NIMP| Simona ICONARU, Author at NIMP

Publications

1. Biocompatibility and Osteogenic Activity of Samarium-Doped Hydroxyapatite-Biomimetic Nanoceramics for Bone Regeneration Applications

Authors: Balas, M; Badea, MA; Ciobanu, SC; Piciu, F; Iconaru, SL; Dinischiotu, A; Predoi, D

Published: JUN 2024, BIOMIMETICS, 9, 309, DOI: 10.3390/biomimetics9060309

In this study, we report on the development of hydroxyapatite (HAp) and samarium-doped hydroxyapatite (SmHAp) nanoparticles using a cost-effective method and their biological effects on a bone-derived cell line MC3T3-E1. The physicochemical and biological features of HAp and SmHAp nanoparticles are explored. The X-ray diffraction (XRD) studies revealed that no additional peaks were observed after the integration of samarium (Sm) ions into the HAp structure. Valuable information regarding the molecular structure and morphological features of nanoparticles were obtained by using Fourier-transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The elemental composition obtained by using energy-dispersive X-ray spectroscopy (EDS) confirmed the presence of the HAp constituent elements, Ca, O, and P, as well as the presence and uniform distribution of Sm3+ ions. Both HAp and SmHAp nanoparticles demonstrated biocompatibility at concentrations below 25 mu g/mL and 50 mu g/mL, respectively, for up to 72 h of exposure. Cell membrane integrity was preserved following treatment with concentrations up to 100 mu g/mL HAp and 400 mu g/mL SmHAp, confirming the role of Sm3+ ions in enhancing the cytocompatibility of HAp. Furthermore, our findings reveal a positive, albeit limited, effect of SmHAp nanoparticles on the actin dynamics, osteogenesis, and cell migration compared to HAp nanoparticles. Importantly, the biological results highlight the potential role of Sm3+ ions in maintaining cellular balance by mitigating disruptions in Ca2+ homeostasis induced by HAp nanoparticles. Therefore, our study represents a significant contribution to the safety assessment of both HAp and SmHAp nanoparticles for biomedical applications focused on bone regeneration.

2. Sodium bicarbonate-hydroxyapatite used for removal of lead ions from aqueous solution

Authors: Predoi, SA; Ciobanu, SC; Chifiriuc, CM; Iconaru, SL; Predoi, D; Negrila, CC; Marinas, IC; Raaen, S; Rokosz, K; Motelica-Heino, M

Published: JAN 1 2024, CERAMICS INTERNATIONAL, 50, DOI: 10.1016/j.ceramint.2023.10.273

This study reports the development of a novel biocomposite for potential applications in the environmental remediation. The hydroxyapatite/sodium bicarbonate (HAp-SB) biocomposite obtained by a cheap method could offer promising characteristics to be used in environmental applications. The obtaining of HAp-SB ceramic composites was studied with the aim of increasing the adsorption efficiency of lead ions from contaminated waters. A composite material (HAp-SB) with good crystallinity that preserves the hexagonal structure of pure hydroxyapatite was obtained. For the powder recovered after decontamination of the lead solution (PbHAp-SB), the XRD model highlighted additional maxima belonging to Ca10(PO4)5(OH)2, Ca0.805Pb4.195(PO4)(OH) and PbH2P2O7. The FTIR spectra of PbHAp-SB are similar to those of HAp-SB composites showing a broadening of the vibration peaks and a slight shift. The XPS and EDS studies illustrated the purity of the HAp-SB sample. Moreover, the presence of lead in the powder recovered after decontamination was also highlighted by XPS and EDS studies. The efficiency of HAp-SB in the adsorption of Pb2+ ions from the contaminated solution was also highlighted by ultrasound studies using double-distilled water as the reference liquid. The adsorption kinetics were investigated with the aid of Langmuir and Freundlich theoretical models. The results demonstrated that the HAp-SB ceramic composite has a strong affinity for the adsorption of Pb2+ ions from contaminated solutions. The removal efficiency of Pb2+ ions was about 92% for the initial Pb2+ concentration above 50 mg/L. The results of the cell viability and cytotoxicity studies demonstrated that HAp-SB nanoparticles did not influence negatively the HeLa cell's viability and did not induce any significant changes of the morphological features of HeLa cells after 24 h of incubation. The batch adsorption results as well as the cytotoxicity assay results suggested that the HAp-SB powder could be successfully used for the removal of Pb2+ from contaminated water.

3. Physico-Chemical and Antimicrobial Features of Magnesium Doped Hydroxyapatite Nanoparticles in Polymer Matrix

Authors: Ciobanu, SC; Iconaru, SL; Predoi, MV; Ghegoiu, L; Badea, ML; Predoi, D; Jiga, G

Published: AUG 2024, MACROMOLECULAR SYMPOSIA, 413, 2400022, DOI: 10.1002/masy.202400022

Magnesium doped hydroxyapatite nanoparticles in dextran matrix (7MgHApDx) with average size diameter of 18.2 +/- 0.5 nm are synthesized by co-precipitation. The surface morphology and shape of 7MgHApDx particles are established by scanning electron microscopy (SEM). The stability that is evaluated by ultrasound measurements and zeta potential reveals a good stability. More than that, the functional groups present in the studied samples are identified by Fourier transform infrared spectroscopy studies. The antimicrobial properties of 7MgHApDx suspensions are determined against Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231 microbial strains.

4. Exploring the physicochemical traits, antifungal capabilities, and 3D spatial complexity of hydroxyapatite with Ag+-Mg2+substitution in the biocomposite thin films

Authors: Predoi, D; Talu, S; Ciobanu, SC; Iconaru, SL; Matos, RS; da Fonseca, HD

Published: SEP 2024, MICRON, 184, 103661, DOI: 10.1016/j.micron.2024.103661

The silver/magnesium doped hydroxyapatite (AgMgHAp, Ca10_ x-yAgxMgy(PO4)6(OH)2, xAg=0.05 and yMg=0.02) nanocomposites coatings were deposited on Si substrate using the dip coating technique. The resulting coatings were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier transform infrared (FTIR-ATR) spectroscopy, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The EDS analysis highlighted the presence of the constitutive elements of the silver/magnesium doped hydroxyapatite (AgMgHAp) nanocomposites coatings. The surface microtexture of the AgMgHAp was assessed by atomic force microscopy (AFM) technique. The AFM data suggested the obtaining of a uniform deposited layer comprised of equally distributed nanoconglomerates. FT -IR studies highlighted the presence of vibrational modes associated with the phosphate and hydroxyl groups. No bands associated with silver or magnesium were observed. The XPS analysis highlighted the presence of the constituent elements of hydroxyapatite (Ca 2p, P 2 s, O 1 s), as well as dopants (Ag 3d, Mg 1 s and Mg 2p). The antifungal evaluation of AgMgHAp coatings was carried out using the Candida albicans ATCC 10231 fungal strain. The results of the antifungal assay revealed that the AgMgHAp coatings exhibited a strong inhibitory antifungal activity. Furthermore, the data highlighted that the AgMgHAp inhibited the development of biofilm on their surface. The results revealed that the antifungal activity of the coating varied based on the duration of incubation. On the other hand, the data also showed that AgMgHAp nanocomposites coatings inhibited the fungal cell adhesion and development from the early stages of the incubation. In addition to morphological analysis, we additionally take advantage of AFM images to investigate and explore the domain of fractal and multifractal analysis applied to the films under evaluation. Our studies indicates that nanocomposite coatings made from AgMgHAp demonstrate strong antifungal properties. Our studies indicates that nanocomposite coatings made from AgMgHAp demonstrate strong antifungal properties. These results suggest the potential of AgMgHAp nanocomposite coatings as a promising solution for developing innovative antifungal devices in biomedical applications.

5. Copper doped hydroxyapatite nanocomposite thin films: synthesis, physico-chemical and biological evaluation

Authors: Ciobanu, CS; Predoi, D; Iconaru, SL; Predoi, MV; Ghegoiu, L; Buton, N; Motelica-Heino, M

Published: 2024 JUL 29 2024, BIOMETALS, DOI: 10.1007/s10534-024-00620-2

Cu-doped hydroxyapatite (CuHAp) thin films were obtained using spin coating method. To make these thin films, CuHAp suspensions obtained by sol-gel method were used. The coatings obtained were thermally treated at 500 degrees C. After the thermal treatment, the thin films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM). Moreover, the stability of the suspensions before being used to obtain the thin films was certified by dynamic light scattering (DLS), zeta potential methods and ultrasound measurements. In the XRD patterns, the peaks associated with hexagonal hydroxyapatite were identified in accordance with JCPDS no. 09-0432. EDS and XPS results confirmed the presence of Cu ions in the samples. Data about the morphological features and chemical composition of CuHAp thin films were obtained by performing scanning electron microscopy (SEM) measurements. Our results suggest that the CuHAp thin films surface is continuous and homogenous. The presence of the functional groups in the CuHAp thin films was confirmed by Fourier-transform infrared spectroscopy (FTIR) and Raman spectroscopy studies. Information about the surface topography of the CuHAp thin films has been obtained using atomic force microscopy (AFM). The AFM images determined that the surface topography of the CuHAp thin layer is homogenous and continuous without presenting any unevenness or fissures. The cytotoxicity of CuHAp thin films was assessed using human gingival fibroblasts (HGF-1) cells. The results of the cell viability assays demonstrated that the thin films presented good biocompatible properties towards the HGF-1 cells. Additionally, the adherence and development of HGF-1 cells on the surface of CuHAp thin films were determined using AFM. The AFM surface topographies highlighted that the CuHAp thin film's surface favored the attachment and proliferation of HGF-1 cells on their surface.

6. New Physico-Chemical Analysis of Magnesium-Doped Hydroxyapatite in Dextran Matrix Nanocomposites

Authors: Predoi, D; Ciobanu, SC; Iconaru, SL; Talu, S; Ghegoiu, L; Matos, RS; da Fonseca, HD; Trusca, R

Published: JAN 2024, POLYMERS, 16, 125, DOI: 10.3390/polym16010125

The new magnesium-doped hydroxyapatite in dextran matrix (10MgHApD) nanocomposites were synthesized using coprecipitation technique. A spherical morphology was observed by scanning electron microscopy (SEM). The X-ray diffraction (XRD) characterization results show hydroxyapatite hexagonal phase formation. The element map scanning during the EDS analysis revealed homogenous distribution of constituent elements of calcium, phosphor, oxygen and magnesium. The presence of dextran in the sample was revealed by Fourier transform infrared (FTIR) spectroscopy. The antimicrobial activity of the 10MgHAPD nanocomposites was assessed by in vitro assays using Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27853, Streptococcus mutans ATCC 25175, Porphyromonas gingivalis ATCC 33277 and Candida albicans ATCC 10231 microbial strains. The results of the antimicrobial assays highlighted that the 10MgHApD nanocomposites presented excellent antimicrobial activity against all the tested microorganisms and for all the tested time intervals. Furthermore, the biocompatibility assays determined that the 10MgHApD nanocomposites did not exhibit any toxicity towards Human gingival fibroblast (HGF-1) cells.

7. Development of Novel Biocomposites with Antimicrobial-Activity-Based Magnesium-Doped Hydroxyapatite with Amoxicillin

Authors: Cimpeanu, C; Predoi, D; Ciobanu, CS; Iconaru, SL; Rokosz, K; Predoi, MV; Raaen, S; Badea, ML

Published: OCT 2024, ANTIBIOTICS-BASEL, 13, 963, DOI: 10.3390/antibiotics13100963

Background/Objectives: A biocomposite based on magnesium-doped hydroxyapatite and enriched with amoxicillin (MgHApOx) was synthesized using the coprecipitation method and is presented here for the first time. Methods: The stability of MgHAp and MgHApOx suspensions was evaluated by ultrasound measurements. The structure of the synthesized MgHAp and MgHApOx was examined with X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The crystalline structure was determined by X-ray diffraction. The FTIR data were collected in the range of 4000-400 cm-1. The morphology of the nanoparticles was evaluated by scanning electron microscopy (SEM). Furthermore, the biocompatible properties of MgHAp, MgHApOx and amoxicillin (Ox) suspensions were assessed using human fetal osteoblastic cells (hFOB 1.19 cell line). The antimicrobial properties of the MgHAp, MgHApOx and Ox suspension nanoparticles were assessed using the standard reference microbial strains Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922 and Candida albicans ATCC 10231. Results: X-ray studies have shown that the biocomposite retains the characteristics of HAp and amoxicillin. The SEM assessment exhibited that the apatite contains particles at nanometric scale with acicular flakes morphology. The XRD and SEM results exhibited crystalline nanoparticles. The average crystallite size calculated from XRD analysis increased from 15.31 nm for MgHAp to 17.79 nm in the case of the MgHApOx sample. The energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analysis highlighted the presence of the constituent elements of MgHAp and amoxicillin. Moreover, XPS confirmed the substitution of Ca2+ ions with Mg2+ and the presence of amoxicillin constituents in the MgHAp lattice. The results of the in vitro antimicrobial assay demonstrated that MgHAp, MgHApOx and Ox suspensions exhibited good antimicrobial activity against the tested microbial strains. The results showed that the antimicrobial activity of the samples was influenced by the presence of the antibiotic and also by the incubation time. Conclusions: The findings from the biological assays indicate that MgHAp and MgHApOx are promising candidates for the development of new biocompatible and antimicrobial agents for biomedical applications.

8. Novel Antimicrobial Agents Based on Zinc-Doped Hydroxyapatite Loaded with Tetracycline

Authors: Iconaru, SL; Predoi, D; Ciobanu, CS; Negrila, CC; Trusca, R; Raaen, S; Rokosz, K; Ghegoiu, L; Badea, ML; Cimpeanu, C

Published: SEP 2024, ANTIBIOTICS-BASEL, 13, 803, DOI: 10.3390/antibiotics13090803

In this paper, we present for the first time the development of zinc-doped hydroxyapatite enriched with tetracycline (ZnHApTe) powders and provide a comprehensive evaluation of their physico-chemical and biological properties. Various techniques such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR) were used for the sample's complex evaluation. Moreover, the biocompatibility of zinc-doped hydroxyapatite (ZnHAp) and ZnHApTe nanoparticles was evaluated with the aid of human fetal osteoblastic cells (hFOB 1.19 cell line). The results of the biological assays suggested that these nanoparticles hold great promise as potential candidates for the future development of novel biocompatible and antimicrobial agents for biomedical applications. The antimicrobial properties of the ZnHAp and ZnHApTe nanoparticles were assessed using the standard reference microbial strains Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231. The results of the in vitro antimicrobial assay demonstrated that both tested materials exhibited good antimicrobial activity. Additionally, these data also indicated that the antimicrobial effects of the ZnHAp nanoparticles were intensified by the presence of tetracycline (Te). Furthermore, the results also suggested that the antimicrobial activity of the samples increased with the incubation time.

9. Physico-Chemical and Biological Features of Fluorine-Substituted Hydroxyapatite Suspensions

Authors: Ciobanu, CS; Predoi, D; Iconaru, SL; Predoi, MV; Rokosz, K; Raaen, S; Negrila, CC; Buton, N; Ghegoiu, L; Badea, ML

Published: JUL 2024, MATERIALS, 17, 3404, DOI: 10.3390/ma17143404

Infections related to orthopedic/stomatology surgery are widely recognized as a significant health concern. Therefore, the development of new materials with superior biological properties and good stability could represent a valuable alternative to the classical treatments. In this paper, the fluorine-substituted hydroxyapatite (FHAp) suspension, with the chemical formula Ca10(PO4)6(OH)2-2xF2x (where x = 0.05), was prepared using a modified coprecipitation technique. Stability studies were conducted by zeta potential and ultrasound measurements for the first time. The X-ray diffraction (XRD) patterns of FHAp powders displayed a hexagonal structure akin to that of pure hydroxyapatite (HAp). The XPS general spectrum revealed peaks corresponding to the constituent elements of fluorine-substituted hydroxyapatite such as calcium, phosphorus, oxygen, and fluorine. The purity of the obtained FHAp samples was confirmed by energy-dispersive X-ray spectroscopy (EDS) studies. The FHAp morphology was evaluated by scanning electron microscopy (SEM) measurements. Fourier-transform infrared spectroscopy (FTIR) studies were performed in order to study the vibrational properties of the FHAp samples. The FHAp suspensions were tested for antibacterial activity against reference strains such as Staphylococcus aureus 25923 ATCC, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231. Additionally, the biocompatibility of the FHAp suspensions was assessed using human fetal osteoblastic cells (hFOB 1.19 cell line). The results of our biological tests suggest that FHAp suspensions are promising candidates for the future development of new biocompatible and antimicrobial agents for use in the biomedical field.

10. A new porous composite hydroxyapatite/chitosan/microcrystalline-cellulose: synthesis, characterization and application to the adsorption of Eriochrome Black T

Authors: Benali, Y; Mabrouki, N; Agougui, H; Jabli, M; Majdoub, H; Predoi, D; Ciobanu, S; Iconaru, SL; Talu, S; Boughzala, K

Published: DEC 2024, POLYMER BULLETIN, 81, DOI: 10.1007/s00289-024-05496-3

In the current study, a porous composite material, hydroxyapatite/chitosan/microcrystalline-cellulose (CaHAp-CS-MCC), was successfully prepared and used for the adsorption of Eriochrome Black T (EBT) from water. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), differential thermal analysis (DTA), thermogravimetric analysis (TGA), specific surface area (SSA), and atomic force microscope (AFM) were used to evaluate the physicochemical properties of the prepared adsorbents. CaHAp-CS-MCC exhibited a decrease in crystallinity and reduction in crystallite size. CaHAp-CS-MCC surface exhibited cracks and pores. AFM displayed changes in surface micro-texture of CaHAp, formation of new surface structures, and variations in particle size and distribution. Upon grafting CaHAp with CS and MCC, its specific surface area decreased from 139.224 to 11.775 m2/g. BET suggested that filling CaHAp pores by CS and MCC contributed to the reduction in surface area. The pore volume values decreased from 2.56 x 10-1 (CaHAp) to 3.91 x 10-2 cm3/g (CaHAp-CS-MCC). Adsorption equilibrium was reached at about 40 min. The adsorption capacities values of CaHAp-CS-MCC and CaHAp were equal to 248 mg/g and 92 mg/g, respectively. The pseudo-second order and the Langmuir equations fitted well the adsorption phenomenon. The calculated thermodynamic parameters showed an exothermic and non-spontaneous system.

11. Synthesis, characterization, and antifungal properties of chrome-doped hydroxyapatite thin films

Authors: Predoi, D; Iconaru, SL; Ciobanu, SC; Predoi, SA; Buton, N; Ramos, GQ; Fonseca, HDD; Fonseca; Matos, RS; Talu, ST

Published: SEP 15 2024, MATERIALS CHEMISTRY AND PHYSICS, 324, 129690, DOI: 10.1016/j.matchemphys.2024.129690

The development of thin films of chromium-doped hydroxyapatite (20CrHAp) deposited on silicon substrate by the spin coating method was realized for the first time. A coherent investigation of the physicochemical properties of 20CrHAp thin films was also carried out for the first time. The obtained thin films were studied by various techniques such as, scanning electron microscopy (SEM), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR) investigations and fractal analysis. By scanning electron microscopy (SEM) studies were obtained valuable information about the surface morphology of the 20CrHAp thin films. The zeta potential (ZP), Dynamic light scattering (DLS) and ultrasound measurements (US) were used in order to evaluate the stability of 20CrHAp suspension. The ratio between the hydrodynamic diameter obtained by DLS and the particle diameter obtained by SEM was 1.6. The SEM results on 20CrHAp thin films suggested that the sample possess a conglomerate of nanoparticles unevenly distributed on their surface. The surface morphology of the 20CrHAp thin films was studied with the aid of atomic force microscopy (AFM). The AFM topography of the 20CrHAp thin film's surface highlighted that the thin films present the morphology of a continuum deposited layer composed of non-uniform particle conglomerates. The presence of hydroxyapatite on the surface of silicium effects on the development of the fungal cells on their surface. Furthermore, our investigation delves into the

12. Physico-Chemical Properties of Copper-Doped Hydroxyapatite Coatings Obtained by Vacuum Deposition Technique

Authors: Benali, Y; Predoi, D; Rokosz, K; Ciobanu, CS; Iconaru, SL; Raaen, S; Negrila, CC; Cimpeanu, C; Trusca, R; Ghegoiu, L; Bleotu, C; Marinas, IC; Stan, M; Boughzala, K

Published: AUG 2024, MATERIALS, 17, 3681, DOI: 10.3390/ma17153681

The hydroxyapatite and copper-doped hydroxyapatite coatings (Ca10-xCux(PO4)6(OH)2; xCu = 0, 0.03; HAp and 3CuHAp) were obtained by the vacuum deposition technique. Then, both coatings were analyzed by the X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and water contact angle techniques. Information regarding the in vitro antibacterial activity and biological evaluation were obtained. The XRD studies confirmed that the obtained thin films consist of a single phase associated with hydroxyapatite (HAp). The obtained 2D and 3D SEM images did not show cracks or other types of surface defects. The FTIR studies' results proved the presence of vibrational bands characteristic of the hydroxyapatite structure in the studied coating. Moreover, information regarding the HAp and 3CuHAp surface wettability was obtained by water contact angle measurements. The biocompatibility of the HAp and 3CuHAp coatings was evaluated using the HeLa and MG63 cell lines. The cytotoxicity evaluation of the coatings was performed by assessing the cell viability through the MTT assay after incubation with the HAp and 3CuHAp coatings for 24, 48, and 72 h. The results proved that the 3CuHAp coatings exhibited good biocompatible activity for all the tested intervals. The ability of Pseudomonas aeruginosa 27853 ATCC (P. aeruginosa) cells to adhere to and develop on the surface of the HAp and 3CuHAp coatings was investigated using AFM studies. The AFM studies revealed that the 3CuHAp coatings inhibited the formation of P. aeruginosa biofilms. The AFM data indicated that P. aeruginosa's attachment and development on the 3CuHAp coatings were significantly inhibited within the first 24 h. Both the 2D and 3D topographies showed a rapid decrease in attached bacterial cells over time, with a significant reduction observed after 72 h of exposure. Our studies suggest that 3CuHAp coatings could be suitable candidates for biomedical uses such as the development of new antimicrobial agents.

13. Morphological and fractal features of cancer cells anchored on composite layers based on magnesium-doped hydroxyapatite loaded in chitosan matrix

Authors: Talu, S; Matos, RS; da Fonseca, HD; Predoi, D; Iconaru, SL; Ciobanu, CS; Ghegoiu, L

Published: JAN 2024, MICRON, 176, 103548, DOI: 10.1016/j.micron.2023.103548

In the present study, we report the development and characterization of composite layers (by spin coating) based on magnesium-doped hydroxyapatite in a chitosan matrix, containing human osteosarcoma MG63 cells anchored. Studies regarding the biocompatibility of the composite layers were performed with the aid of a MTT (3-4,5-Dimethylthiazol 2,5-diphenyltetrazolium bromide) assay. The data determined that the composite layers did not inhibit the growth and adhesion of MG63 cells to their surfaces exhibiting good biocompatibility properties. Furthermore, the attachment and development of MG63 cells on the surface of MgHApCh composite layers were investigated using atomic force microscopy (AFM). AFM topographical maps emphasized that the HApCh and 8MgHApCh composite layers surface promoted the attachment and proliferation of MG63 cells on their surface. Meanwhile, in the case of 30MgHApCh layers incubated for 48 h, a slight modification of the morphological features of the MG63 cells. In addition, the effects of the composite layers against Candida albicans ATCC 10231 were also evaluated. The data results from the in vitro antifungal assay depicted that the composite layers successfully inhibited the growth of the fungal cells onto their surface. Morphological and fractal analyses unveil cancer cell surfaces on Mg-containing composite layers with intricate 3D patterns, driven by highfrequency components. Their remarkable complexity and roughness arises from a strong multifractal nature, supporting more effective vertical growth compared to Si and HApCh surfaces. The cell viability reduced of uncoated Si surface is highlighted by its less intense 3D pattern growth. Our results show that the uncoated Si surface promotes lower viability of MG63 cancer cells, with less rough and complex 3D spatial patterns.

14. Hydroxyapatite Nanopowders for Effective Removal of Strontium Ions from Aqueous Solutions

Authors: Predoi, SA; Ciobanu, SC; Chifiriuc, MC; Motelica-Heino, M; Predoi, D; Iconaru, SL

Published: JAN 2023, MATERIALS, 16, 229, DOI: 10.3390/ma16010229

Drinking water contamination has become a worldwide problem due to the highly negative effects that pollutants can have on human organisms and the environment. Hydroxyapatite (HAp) has the appropriate properties for the immobilization of various pollutants, being considered amongst the most cost-effective materials for water decontamination. The main objective of this study was to use synthesized hydroxyapatite for the elimination of Sr2+ ions from contaminated solutions. The hydroxyapatite used in the decontamination process was synthesized in the laboratory using an adapted method. The hydroxyapatite powder (HAp) resulting from the synthesis was analyzed both before and after the elimination of Sr2+ ions from contaminated solutions. The efficiency of the HAp nanoparticles in removing Sr2+ ions from contaminated solution was determined by batch adsorption experiments. X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were used to study the HAp samples before and after the removal of Sr2+ ions. The ability of HAp nanoparticles to eliminate strontium ions from contaminated solutions was established. Moreover, the removal of Sr2+ ions from the contaminated aqueous solutions was highlighted by ultrasound measurements. The value of the stability parameter calculated by ultrasonic measurements after the removal of Sr2+ ions from the contaminated solution was similar to that of double distilled water whose stability was used as reference. The outcomes of the batch experiments and the parameters obtained from Langmuir and Freundlich models indicated that the HAp nanoparticles had a strong affinity for the elimination of Sr2+ ions from polluted solutions. These results emphasized that HAp nanoparticles could be excellent candidates in the development of new technologies for water remediation. More than that, the outcomes of the cytotoxic assays proved that HAp nanoparticles did not induce any noticeable harmful effects against HeLa cells and did not affect their proliferation after 1 day and 7 days of incubation.

15. Salvia officinalis-Hydroxyapatite Nanocomposites with Antibacterial Properties

Authors: Ciobanu, SC; Predoi, D; Chifiriuc, MC; Iconaru, SL; Predoi, MV; Popa, M; Rokosz, K; Raaen, S; Marinas, IC; Huang, HM

Published: DEC 2023, POLYMERS, 15, 4484, DOI: 10.3390/polym15234484

In the present study, sage-coated zinc-doped hydroxyapatite was incorporated into a dextran matrix (7ZnHAp-SD), and its physico-chemical and antimicrobial activities were investigated. A 7ZnHAp-SD nanocomposite suspension was obtained using the co-precipitation method. The stability of the nanocomposite suspension was evaluated using ultrasound measurements. The stability parameter calculated relative to double-distilled water as a reference fluid highlights the very good stability of the 7ZnHAp-SD suspension. X-ray diffraction (XRD) experiments were performed to evaluate the characteristic diffraction peak of the hydroxyapatite phase. Valuable information regarding the morphology and chemical composition of 7ZnHAp-SD was obtained via scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS) studies. Fourier-transform infrared spectroscopy (FTIR) measurements were performed on the 7ZnHAp-SD suspensions in order to evaluate the functional groups present in the sample. Preliminary studies on the antimicrobial activity of 7ZnHAp-SD suspensions against the standard strains of Staphylococcus aureus 25923 ATCC, Enterococcus faecalis 29212 ATCC, Escherichia coli 25922 ATCC, and Pseudomonas aeruginosa 27853 ATCC were conducted. More than that, preliminary studies on the biocompatibility of 7ZnHAp-SD were conducted using human cervical adenocarcinoma (HeLa) cells, and their results emphasized that the 7ZnHAp-SD sample did not exhibit a toxic effect and did not induce any noticeable changes in the morphological characteristics of HeLa cells. These preliminary results showed that these nanoparticles could be possible candidates for biomedical/antimicrobial applications.

16. Influence of the Biological Medium on the Properties of Magnesium Doped Hydroxyapatite Composite Coatings

Authors: Predoi, D; Ciobanu, SC; Iconaru, SL; Predoi, MV

Published: FEB 2023, COATINGS, 13, 409, DOI: 10.3390/coatings13020409

In this paper, the stability of magnesium-doped hydroxyapatite/chitosan (MHC) suspension obtained with the sol-gel approach was evaluated using nondestructive ultrasound measurements. The MHC coatings obtained by the spin-coating technique were characterized before and after immersion for 7 and 14 days, respectively, in Dulbecco's modified eagle medium (DMEM) by scanning electron microscopy, equipped with an EDAX detector. Also, the functional groups present on the MHC coatings surface were analyzed with the aid of attenuated total reflection (ATR) Fourier transform infrared (FTIR) spectroscopy. The surface microstructure was evaluated using two commentary techniques, namely atomic force microscopy (AFM) and metallographic microscopy (MM). The influence of immersion in DMEM on the biological properties was studied with in vitro studies using primary osteoblast and HCT-8 cell lines. Our results revealed that both surface morphology and chemical composition of the MHC coatings allow rapid development of a new apatite layer on their surface after immersion in DMEM. Preliminary in vitro biological studies underlined the noncytotoxic effect of the studied samples on the proliferation of primary osteoblast and HCT-8 cell lines, which makes them a promising candidate for applications in fields such as orthopedics or dentistry. The antifungal assay of the MHC coatings was assessed using Candida albicans ATCC 10231 and their results showed a good inhibitory effect. The coatings made on the basis of the MHC composite could contribute to increasing the degree of success of implants by decreasing the risk of infections and postoperative inflammation.

17. In Vitro and In Vivo Biological Assays of Dextran Coated Iron Oxide Aqueous Magnetic Fluids

Authors: Predoi, SA; Iconaru, SL; Predoi, D

Published: JAN 2023, PHARMACEUTICS, 15, 177, DOI: 10.3390/pharmaceutics15010177

The iron oxide nanoparticles coated with different surface coatings were studied and characterized by multiple physicochemical and biological methods. The present paper aims at estimating the toxicity in vitro and in vivo of dextran coated iron oxide aqueous magnetic fluids. The in vitro studies were conducted by quantifying the viability of HeLa cells after their incubation with the samples (concentrations of 62.5-125-250-500 mu g/mL at different time intervals). The estimation of the toxicity in vivo of administering dextran coated iron oxide aqueous magnetic fluids (DIO-AMF) with hydrodynamic diameter of 25.73 +/- 4 nm to Male Brown Norway rats has been made. Different concentrations (62.5-125-250-500 mu g/mL) of dextran coated iron oxide aqueous magnetic fluids were administered for 7 consecutive days. Hematology and biochemistry of the Male Brown Norway rats assessment was performed at various time intervals (24-72 h and 21-28 days) after intra-peritoneal injection. The results showed that high concentrations of DIO-AMF (250 and 500 mu g/mL) significantly increased white blood cells, red blood cells, hemoglobin and hematocrit compared to the values obtained for the control group (p < 0.05). Moreover, following the administration of DIO-AMF, the levels of alkaline phosphatase and aspartate aminotransferase increased compared to the control group (p < 0.05). After DIO-AMF administration, no significant difference was observed in the levels of alanine aminotransferase, gamma-glutamyl transpeptidase, urea and creatinine compared to the control group (p < 0.05). The results of the present study showed that dextran coated iron oxide aqueous magnetic fluids in concentrations lower than 250 mu g/mL are reliable for medical and pharmaceutical applications.

18. Complex Evaluation of Nanocomposite-Based Hydroxyapatite for Biomedical Applications

Authors: Predoi, D; Iconaru, SL; Ciobanu, SC; Buton, N; Predoi, MV

Published: NOV 2023, BIOMIMETICS, 8, 528, DOI: 10.3390/biomimetics8070528

A magnesium-doped hydroxyapatite in chitosan matrix (MgHApC) sample was developed as a potential platform for numerous applications in the pharmaceutical, medical, and food industries. Magnesium-doped hydroxyapatite suspensions in the chitosan matrix were obtained by the coprecipitation technique. The surface shape and morphological features were determined by scanning electron microscopy (SEM). The hydrodynamic diameter of the suspended particles was determined by Dynamic light scattering (DLS) measurements. The stability of MgHApC suspensions was evaluated by ultrasonic measurements. The hydrodynamic diameter of the MgHApC particles in suspension was 29.5 nm. The diameter of MgHApC particles calculated from SEM was 12.5 +/- 2 nm. Following the SEM observations, it was seen that the MgHApC particles have a spherical shape. The Fourier-transform infrared spectroscopy (FTIR) studies conducted on MgHApC proved the presence of chitosan and hydroxyapatite in the studied specimens. In vitro antimicrobial assays were performed on Escherichia coli ATCC 25922, Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27853, and Candida albicans ATCC 10231 microbial strains. The antimicrobial experiments showed that MgHApC exhibited very good antimicrobial properties against all the tested microorganisms. More than that, the results of the in vitro studies revealed that the antimicrobial properties of the samples depend on the incubation time. The evaluation of the sample's cytotoxicity was performed using the human colon cancer (HCT-8) cell line. Our results suggested the great potential of MgHApC to be used in future applications in the field of biomedical applications (e.g., dentistry, orthopedics, etc.).

19. Development of Novel Tetracycline and Ciprofloxacin Loaded Silver Doped Hydroxyapatite Suspensions for Biomedical Applications

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Buton, N

Published: JAN 2023, ANTIBIOTICS-BASEL, 12, 74, DOI: 10.3390/antibiotics12010074

The objective of this study consisted of the development of new materials with antimicrobial properties at the nanometric scale that could lead to an increase in therapeutic efficacy and reduction of toxic side effects. This work focuses on obtaining and characterizing stable suspensions with narrow size distribution with antimicrobial properties. The stability of the suspensions obtained by an adapted co-precipitation method was evaluated by ultrasonic measurements. The size and size distribution of the particle populations were determined using scanning electron microscopy (SEM), and dynamic light scattering (DLS). Both methods of analysis showed a narrow distribution of particles. DLS gave a monomodal distribution with hydrodynamic diameters around 38 nm for ciprofloxacin embedded in silver doped hydroxyapatite (AgHA-C) and 45.7 nm for tetracycline embedded in silver doped hydroxyapatite (AgHA-T). The average diameters calculated from SEM were 17 nm for AgHA-C and 19 nm for AgHA-T. Both Ciprofloxacin and Tetracycline influenced the hydroxyapatite structure, which led to the appearance of new vibrational bands characteristic of the specific chemical composition in the FTIR spectrum. The antimicrobial properties of the AgHA-C and AgHA-T suspensions were assessed using the most common reference microbial strains Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231. The results of the in vitro antimicrobial assays determined that the AgHA-C and AgHA-T suspensions exhibited exceptional antimicrobial activity. Moreover, the data revealed that the antimicrobial activity increased with the increase of the incubation time.

20. Response of the Endogenous Antioxidant Defense System Induced in RAW 264.7 Macrophages upon Exposure to Dextran-Coated Iron Oxide Nanoparticles

Authors: Balas, M; Iconaru, SL; Dinischiotu, A; Buton, N; Predoi, D

Published: FEB 2023, PHARMACEUTICS, 15, 552, DOI: 10.3390/pharmaceutics15020552

Presently, iron oxide nanoparticles are the only ones approved for clinical use as contrast agents in magnetic resonance imaging (MRI). Even though there is a high demand for these types of nanoparticles both for clinical use as well as for research, there are difficulties in obtaining stable nanoparticles with reproducible properties. In this context, in this study, we report the obtaining by an adapted coprecipitation method of dextran-coated maghemite nanoparticles (gamma-Fe2O3 NPs). The morphology and structure of the dextran-coated maghemite nanoparticles (gamma-Fe2O3 NPs) were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The TEM and SEM micrographs highlighted the obtaining of particles of nanometric size and spherical shape morphology. Furthermore, the high-resolution transmission electron microscopy (HRTEM), as well as selected area diffraction (SAED), revealed that the obtained samples presented the structure of cubic maghemite. In this study, we also explored the effects of the co-precipitation synthesized dextran-coated maghemite nanoparticles (gamma-Fe2O3 NPs) on the redox status of macrophages. For cytotoxicity evaluation of these NPs, murine macrophages (RAW 264.7 cell line) were exposed to different concentrations of dextran-coated maghemite nanoparticles (gamma-Fe2O3 NPs) corresponding to 0-500 mu g Fe3+/mL and incubated for 24, 48, and 72 h. Intracellular iron uptake, changes in the oxidative stress parameters (reactive oxygen species production and malondialdehyde level), and the activity of antioxidant enzymes, as well as GSH concentration in cells, were evaluated after incubation with a lower (50 mu g Fe3+/mL) and higher (500 mu g Fe3+/mL) dose of NPs. The results indicated a significant decrease in RAW 264.7 cell viability after 72 h in the presence of NPs at concentrations above 25 mu g Fe3+/mL. An important accumulation of NPs, dependent on dose and exposure time, was detected in macrophages, but it induced only a limited raise in the oxidative status. We showed here that the antioxidant capacity of RAW 264.7 macrophages was efficient in counteracting dextran-coated maghemite nanoparticles (gamma-Fe2O3 NPs) toxicity even at higher doses.

21. Biocomposite Coatings Doped with Magnesium and Zinc Ions in Chitosan Matrix for Antimicrobial Applications

Authors: Predoi, D; Ciobanu, CS; Iconaru, SL; Raaen, S; Rokosz, K

Published: JUN 2023, MATERIALS, 16, 4412, DOI: 10.3390/ma16124412

Hydroxyapatite doped with magnesium and zinc in chitosan matrix biocomposites have great potential for applications in space technology, aerospace, as well as in the biomedical field, as a result of coatings with multifunctional properties that meet the increased requirements for wide applications. In this study, coatings on titanium substrates were developed using hydroxyapatite doped with magnesium and zinc ions in a chitosan matrix (MgZnHAp_Ch). Valuable information concerning the surface morphology and chemical composition of MgZnHAp_Ch composite layers were obtained from studies that performed scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), metallographic microscopy, and atomic force microscopy (AFM). The wettability of the novel coatings, based on magnesium and zinc-doped biocomposites in a chitosan matrix on a titanium substrate, was evaluated by performing water contact angle studies. Furthermore, the swelling properties, together with the coating's adherence to the titanium substrate, were also analyzed. The AFM results emphasized that the composite layers exhibited the surface topography of a uniform layer, and that there were no evident cracks and fissures present on the investigated surface. Moreover, antifungal studies concerning the MgZnHAp_Ch coatings were also carried out. The data obtained from quantitative antifungal assays highlight the strong inhibitory effects of MgZnHAp_Ch against C. albicans. Additionally, our results underline that after 72 h of exposure, the MgZnHAp_Ch coatings display fungicidal features. Thus, the obtained results suggest that the MgZnHAp_Ch coatings possess the requisite properties that make them suitable for use in the development of new coatings with enhanced antifungal features.

22. Studies of New Layer Formation on the Surface of Zinc Doped Hydroxyapatite/Chitosan Composite Coatings in Biological Medium

Authors: Motelica-Heino, M; Predoi, MV; Ciobanu, SC; Iconaru, SL; Predoi, D

Published: FEB 2023, COATINGS, 13, 472, DOI: 10.3390/coatings13020472

Usually, before being used in biomedical applications, a biomaterials' bioactivity is tested by in vitro methods that simulate similar conditions to those found in the human body. In this work, we report on the synthesis of zinc-doped hydroxyapatite-chitosan (ZnHApC) composite coatings by the vacuum deposition method. The surface microstructure and the chemical and molecular modification of the coatings before and after soaking in DMEM (Dulbecco's Modified Eagle's Medium) were studied. For this objective, techniques such as attenuated total reflection (ATR), Fourier transform infrared (FTIR) spectroscopy, metallographic microscopy (MM), and scanning electron microscopy (SEM) were applied used. Also, water contact angle measurements and swelling studies were made on ZnHApC composite coatings before and after soaking in a biological medium. The coatings' adherence to the substrate was also studied. The results of antifungal studies on ZnHApC composite coatings against the Candida albicans microbial strain reveal their good antifungal activity. The biocompatibility of the composite coatings was tested using a primary osteoblast cell line. Our results suggest that zinc-doped hydroxyapatite-chitosan samples could be used as a bioimplant material due to their enhanced bioactivity and biocompatibility.

23. Studies of the Tarragon Essential Oil Effects on the Characteristics of Doped Hydroxyapatite/Chitosan Biocomposites

Authors: Predoi, D; Iconaru, SL; Ciobanu, CS; Raita, MS; Ghegoiu, L; Trusca, R; Badea, ML; Cimpeanu, C

Published: APR 2023, POLYMERS, 15, 1908, DOI: 10.3390/polym15081908

Due to the emergence of antibiotic-resistant pathogens, the need to find new, efficient antimicrobial agents is rapidly increasing. Therefore, in this study, we report the development of new biocomposites based on zinc-doped hydroxyapatite/chitosan enriched with essential oil of Artemisia dracunculus L. with good antimicrobial activity. Techniques such as scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FTIR) were used in order to evaluate their physico-chemical properties. Our studies revealed that biocomposite materials with nanometric dimension and homogeneous composition could be obtained through an economic and cost-effective synthesis method. The biological assays demonstrated that ZnHA (zinc-doped hydroxyapatite), ZnHACh (zinc-doped hydroxyapatite/chitosan) and ZnHAChT (zinc-doped hydroxyapatite/chitosan enriched with essential oil of Artemisia dracunculus L.) did not exhibit a toxic effect on the cell viability and proliferation of the primary osteoblast culture (hFOB 1.19). Moreover, the cytotoxic assay also highlighted that the cell morphology of the hFOB 1.19 was not altered in the presence of ZnHA, ZnHACh or ZnHAChT. Furthermore, the in vitro antimicrobial studies emphasized that the samples exhibited strong antimicrobial properties against Escherichia coli ATCC 25922, Staphylococcus aureus ATCC 25923 and Candida albicans ATCC 10231 microbial strains. These results are encouraging for the following development of new composite materials with enhanced biological properties that could promote the osteogenic process of bone healing and also exhibit good antimicrobial properties.

24. Novel Dextran Coated Cerium Doped Hydroxyapatite Thin Films

Authors: Ciobanu, CS; Nica, IC; Dinischiotu, A; Iconaru, SL; Chapon, P; Bita, B; Trusca, R; Groza, A; Predoi, D

Published: MAY 2022, POLYMERS, 14, 1826, DOI: 10.3390/polym14091826

Dextran coated cerium doped hydroxyapatite (Ca(10-x)Cex(PO4)(6)(OH)(2)), with x = 0.05 (5CeHAp-D) and x = 0.1 (10CeHAp-D) were deposited on Si substrates by radio frequency magnetron sputtering technique for the first time. The morphology, composition, and structure of the resulting coatings were examined by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), atomic force microscopy (AFM), metallographic microscopy (MM), Fourier transform infrared spectroscopy (FTIR), and glow discharge optical emission spectroscopy (GDOES), respectively. The obtained information on the surface morphologies, composition and structure was discussed. The surface morphologies of the CeHAp-D composite thin films are smooth with no granular structures. The constituent elements of the CeHAp-D target were identified. The results of the FTIR measurements highlighted the presence of peaks related to the presence of nu(1), nu(3), and nu(4) vibration modes of (PO43-) groups from the hydroxyapatite (HAp) structure, together with those specific to the dextran structure. The biocompatibility assessment of 5CeHAp-D and 10CeHAp-D composite coatings was also discussed. The human cells maintained their specific elongated morphology after 24 h of incubation, which confirmed that the behavior of gingival fibroblasts and their proliferative capacity were not disturbed in the presence of 5CeHAp-D and 10CeHAp-D composite coatings. The 5CeHAp-D and 10CeHAp-D coatings' surfaces were harmless to the human gingival fibroblasts, proving good biocompatibility.

25. Development of Silver Doped Hydroxyapatite Thin Films for Biomedical Applications

Authors: Iconaru, SL; Predoi, D; Ciobanu, CS; Motelica-Heino, M; Guegan, R; Bleotu, C

Published: MAR 2022, COATINGS, 12, 341, DOI: 10.3390/coatings12030341

Silver doped hydroxyapatite [AgHAp, Ca10-xAg(PO4)(6)(OH)(2)], due to its antimicrobial properties, is an advantageous material to be used for various coatings. The AgHAp thin films with x(Ag) = 0.05 and x(Ag) = 0.1 were achieved using the spin-coating method. The resulting samples were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). XRD analysis revealed that the particles of both samples are ellipsoidal. Also, in agreement with the results obtained by XRD measurements, the results of the SEM studies have shown that the particles shape is ellipsoidal. Optical properties of silver doped hydroxyapatite thin films deposited on Si substrate were investigated through Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. The results obtained by the two complementary techniques highlighted that the molecular structure of the studied samples is not influenced by the increase of the silver concentration in the samples. Our studies revealed that the surface morphology of the obtained samples consist of uniform and continuous layers. The biocompatibility of the obtained thin films was also evaluated with the aid of human osteosarcoma MG63 (ATCC CRL 1427) cell line. Moreover, the in vitro antifungal activity against Candida albicans fungal strain of the AgHAp thin films was studied and the obtained results revealed their antifungal effect. The results of the biological assays showed that the AgHAp thin films are a very promising material for biomedical applications.

26. Impact of Gamma Irradiation on the Properties of Magnesium-Doped Hydroxyapatite in Chitosan Matrix

Authors: Predoi, D; Ciobanu, CS; Iconaru, SL; Predoi, SA; Chifiriuc, MC; Raaen, S; Badea, ML; Rokosz, K

Published: AUG 2022, MATERIALS, 15, 5372, DOI: 10.3390/ma15155372

This is the first report regarding the effect of gamma irradiation on chitosan-coated magnesium-doped hydroxyapatite (x(Mg) = 0.1; 10 MgHApCh) layers prepared by the spin-coating process. The stability of the resulting 10 MgHApCh gel suspension used to obtain the layers has been shown by ultrasound measurements. The presence of magnesium and the effect of the irradiation process on the studied samples were shown by X-ray photoelectron spectroscopy (XPS). The XPS results obtained for irradiated 10 MgHApCh layers suggested that the magnesium and calcium contained in the surface layer are from tricalcium phosphate (TCP; Ca-3(PO4)(2)) and hydroxyapatite (HAp). The XPS analysis has also highlighted that the amount of TCP in the surface layer increased with the irradiation dose. The energy-dispersive X-ray spectroscopy (EDX) evaluation showed that the calcium decreases with the increase in the irradiation dose. In addition, a decrease in crystallinity and crystallite size was highlighted after irradiation. By atomic force microscopy (AFM) we have obtained images suggesting a good homogeneity of the surface of the non-irradiated and irradiated layers. The AFM results were also sustained by the scanning electron microscopy (SEM) images obtained for the studied samples. The effect of gamma-ray doses on the Fourier transform infrared spectroscopy (ATR-FTIR) spectra of 10 MgHApCh composite layers was also evaluated. The in vitro antifungal assays proved that 10 MgHApCh composite layers presented a strong antifungal effect, correlated with the irradiation dose and incubation time. The study of the stability of the 10 MgHApCh gel allowed us to achieve uniform and homogeneous layers that could be used in different biomedical applications.

27. Physicochemical Characterization of Europium-Doped Hydroxyapatite Thin Films with Antifungal Activity

Authors: Ciobanu, CS; Predoi, MV; Buton, N; Megier, C; Iconaru, SL; Predoi, D

Published: MAR 2022, COATINGS, 12, 306, DOI: 10.3390/coatings12030306

Owing to its unique biological and physicochemical properties, hydroxyapatite (HAp) represents one of the most extensively studied biomaterials for biomedical applications. It is well known that Candida is currently one of the fungi frequently involved in the onset and development of post-implant infections and, owing to the appearance of antifungal resistance, it is quite difficult to treat despite all the tremendous efforts made in this regard by the scientific world. Therefore, in this context, we report for the first time in this paper, the development and characterization of europium-doped thin films (5EuHAp, x(Eu) = 0.05) on a Si substrate by a spin-coating method. The results of ultrasound (US), zeta (zeta) potential, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and Fourier-transform infrared spectroscopy (FTIR) studies are presented. The XRD studies conducted on 5EuHAp suspension revealed the nanometric dimensions of the particles and sample purity. In addition, a moderate stability of the 5EuHAp suspension was observed. XPS measurements revealed the presence of Eu 3d in the 5EuHAp thin films. In the SEM micrographs, the surface uniformity and the absence of the surface defects could be observed. Moreover, the results of the FTIR studies showed the presence of the vibrational bands specific to the HAp structure in the studied sample. The antifungal activity of the HAp and 5EuHAp suspensions and coatings was evaluated using the Candida albicans ATCC 10231 (C. albicans) fungal strain. The qualitative assays of the antifungal properties of HAp and 5EuHAp coatings were also visualized by SEM and CLSM. The antifungal studies revealed that both 5EuHAp suspensions and coatings exhibited noticeable antifungal activity against C. albicans cells.

28. The Effects of Electron Beam Irradiation on the Morphological and Physicochemical Properties of Magnesium-Doped Hydroxyapatite/Chitosan Composite Coatings

Authors: Bita, B; Stancu, E; Stroe, D; Dumitrache, M; Ciobanu, SC; Iconaru, SL; Predoi, D; Groza, A

Published: FEB 2022, POLYMERS, 14, 582, DOI: 10.3390/polym14030582

This work reports on the influence of 5 MeV electron beam radiations on the morphological features and chemical structure of magnesium-doped hydroxyapatite/chitosan composite coatings generated by the magnetron sputtering technique. The exposure to ionizing radiation in a linear electron accelerator dedicated to medical use has been performed in a controllable manner by delivering up to 50 Gy radiation dose in fractions of 2 Gy radiation dose per 40 s. After the irradiation with electron beams, the surface of layers became nano-size structured. The partial detachment of irradiated layers from the substrates has been revealed only after visualizing their cross sections by scanning electron microscopy. The energy dispersive X-ray spectral analysis of layer cross-sections indicated that the distribution of chemical elements in the samples depends on the radiation dose. The X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction analysis have shown that the physicochemical processes induced by the ionizing radiation in the magnesium doped hydroxyapatite/chitosan composite coatings do not alter the apatite structure, and Mg remains bonded with the phosphate groups.

29. Physicochemical and Biological Evaluation of Chitosan-Coated Magnesium-Doped Hydroxyapatite Composite Layers Obtained by Vacuum Deposition

Authors: Predoi, D; Ciobanu, CS; Iconaru, SL; Raaen, S; Badea, ML; Rokosz, K

Published: MAY 2022, COATINGS, 12, 702, DOI: 10.3390/coatings12050702

In the present work, the effectiveness of vacuum deposition technique for obtaining composite thin films based on chitosan-coated magnesium-doped hydroxyapatite Ca10-xMgx(PO4)(6) (OH)(2) with x(Mg) = 0.025 (MgHApCh) was proved for the first time. The prepared samples were exposed to three doses (0, 3, and 6 Gy) of gamma irradiation. The MgHApCh composite thin films nonirradiated and irradiated were evaluated by scanning electron microscopy (SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) studies. The biological evaluation of the samples was also presented. All the results obtained from this study showed that the vacuum deposition method allowed for obtaining uniform and homogeneous layers. Fine cracks were observed on the MgHApCh composite thin films' surface after exposure to a 6 Gy irradiation dose. Additionally, after gamma irradiation, a decrease in Ca, P, and Mg content was noticed. The MgHApCh composite thin films with doses of 0 and 3 Gy of gamma irradiation showed a cellular viability similar to that of the control. Samples with 6 Gy doses of gamma irradiation did not cause significantly higher fibroblast cell death than the control (p > 0.05). On the other hand, the homogeneous distribution of pores that appeared on the surface of coatings after 6 Gy doses of gamma irradiation did not prevent the adhesion of fibroblast cells and their spread on the coatings. In conclusion, we could say that the thin films could be suitable both for use in bone implants and for other orthopedic and dentistry applications.

30. Iron-Oxide-Nanoparticles-Doped Polyaniline Composite Thin Films

Authors: Butoi, B; Ciobanu, CS; Iconaru, SL; Negrila, CC; Badea, MA; Balas, M; Dinischiotu, A; Predoi, G; Bita, B; Groza, A; Predoi, D

Published: MAY 2022, POLYMERS, 14, 1821, DOI: 10.3390/polym14091821

Iron-oxide-doped polyaniline (PANI-IO) thin films were obtained by the polymerization of aniline monomers and iron oxide solutions in direct current glow discharge plasma in the absence of a buffer gas for the first time. The PANI-IO thin films were deposited on optical polished Si wafers in order to study surface morphology and evaluate their in vitro biocompatibility. The characterization of the coatings was accomplished using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), metallographic microscopy (MM), and X-ray photoelectron spectroscopy (XPS). In vitro biocompatibility assessments were also conducted on the PANI-IO thin films. It was observed that a uniform distribution of iron oxide particles inside the PANI layers was obtained. The constituent elements of the coatings were uniformly distributed. The Fe-O bonds were associated with magnetite in the XPS studies. The surface morphology of the PANI-IO thin films was assessed by atomic force microscopy (AFM). The AFM topographies revealed that PANI-IO exhibited the morphology of a uniformly distributed and continuous layer. The viability of Caco-2 cells cultured on the Si substrate and PANI-IO coating was not significantly modified compared to control cells. Moreover, after 24 h of incubation, we observed no increase in LDH activity in media in comparison to the control. In addition, our results revealed that the NO levels for the Si substrate and PANI-IO coating were similar to those found in the control sample.

31. Fabrication and Physico-Chemical Properties of Antifungal Samarium Doped Hydroxyapatite Thin Films

Authors: Ciobanu, CS; Predoi, D; Chapon, P; Predoi, MV; Iconaru, SL

Published: DEC 2021, COATINGS, 11, DOI: 10.3390/coatings11121466

Samarium doped hydroxyapatite (Ca10-xSmx(PO4)(6)(OH)(2), x(Sm) = 0.5, 50SmHAp) is a very promising candidate to be used for different coatings in various dental and orthopedic implants. We report, for the first time, the obtaining of 50SmHAp thin films by a cost-effective method, namely spin coating. Thin films of 50SmHAp on silicon substrate have been analyzed by various techniques such as Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), atomic force microscopy (AFM), Metallographic microscopy and Glow Discharge Optical Emission Spectroscopy (GDOES). The stability of 50SmHAp suspension was evaluated by ultrasound measurements. Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were also used to evaluate the 50SmHAp suspension. The antifungal activity of 50SmHAp suspension and coatings was assessed using Candida albicans ATCC 10231 fungal strain (C. albicans). The results of the antifungal assays depicted that both 50SmHAp suspensions and coatings were effective in inhibiting the development of C. albicans fungal cells, thus making them ideal candidates for the development of novel antifungal agents. The obtained results give new perspective for possible applications of 50SmHAp thin films in various medical applications due to their antifungal properties.

32. Preparation of Porous Hydroxyapatite Using Cetyl Trimethyl Ammonium Bromide as Surfactant for the Removal of Lead Ions from Aquatic Solutions

Authors: Predoi, SA; Ciobanu, CS; Motelica-Heino, M; Chifiriuc, MC; Badea, ML; Iconaru, SL

Published: MAY 2021, POLYMERS, 13, DOI: 10.3390/polym13101617

In the present study, a new low-cost bioceramic nanocomposite based on porous hydroxyapatite (HAp) and cetyl trimethyl ammonium bromide (CTAB) as surfactant was successfully obtained by a simple chemical co-precipitation. The composition and structure of the HAp-CTAB were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), scanning electron microscope (SEM) equipped with an energy dispersive X-ray (EDX) spectrometer, and N-2 adsorption/desorption analysis. The capacity of HAp-CTAB nanocomposites to remove the lead ions from aqueous solutions was studied by adsorption batch experiments and proved by Langmuir and Freundlich models. The Pb2+ removal efficiency of HAp-CTAB biocomposite was also confirmed by non-destructive ultrasound studies. The cytotoxicity assays showed that the HAp-CTAB nanocomposites did not induce any significant morphological changes of HeLa cells after 24 h of incubation or other toxic effects. Taken together, our results suggests that the obtained porous HAp-CTAB powder could be used for the decontamination of water polluted with heavy metals, such as Pb2+.

33. Investigation of Spin Coating Cerium-Doped Hydroxyapatite Thin Films with Antifungal Properties

Authors: Iconaru, SL; Predoi, MV; Chapon, P; Gaiaschi, S; Rokosz, K; Raaen, S; Motelica-Heino, M; Predoi, D

Published: APR 2021, COATINGS, 11, DOI: 10.3390/coatings11040464

In this study, the cerium-doped hydroxyapatite (Ca10-xCex(PO4)(6)(OH)(2) with x(Ce) = 0.1, 10Ce-HAp) coatings obtained by the spin coating method were presented for the first time. The stability of the 10Ce-HAp suspension particles used in the preparation of coatings was evaluated by ultrasonic studies, transmission electron microscopy (TEM), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The surface morphology of the 10Ce-HAp coating was studied by SEM and atomic force microscopy (AFM) techniques. The obtained 10Ce-HAp coatings were uniform and without cracks or unevenness. Glow discharge optical emission spectroscopy (GDOES) and X-ray photoelectron spectroscopy (XPS) were used for the investigation of fine chemical depth profiling. The antifungal properties of the HAp and 10Ce-HAp suspensions and coatings were assessed using Candida albicans ATCC 10231 (C. albicans) fungal strain. The quantitative antifungal assays demonstrated that both 10Ce-HAp suspensions and coatings exhibited strong antifungal properties and that they successfully inhibited the development and adherence of C. albicans fungal cells for all the tested time intervals. The scanning electron microscopy (SEM) and confocal laser scanning microscopy (CLSM) visualization of the C. albicans fungal cells adherence to the 10Ce-HAp surface also demonstrated their strong inhibitory effects. In addition, the qualitative assays also suggested that the 10Ce-HAp coatings successfully stopped the biofilm formation.

34. Fabrication of Novel Chitosan-Hydroxyapatite Nanostructured Thin Films for Biomedical Applications

Authors: Ciobanu, CS; Iconaru, SL; Predoi, D; Trusca, RD; Prodan, AM; Groza, A; Chifiriuc, MC; Beuran, M

Published: DEC 2021, COATINGS, 11, DOI: 10.3390/coatings11121561

In this study, we develop chitosan-hydroxyapatite (CS-HAp) composite layers that were deposited on Si substrates in radio frequency (RF) magnetron sputtering discharge in argon gas. The composition and structure of CS-HAp composite layers were investigated by analytical techniques, such as Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), metallographic microscopy (MM), and atomic force microscopy (AFM). On the other hand, in the present study the second order derivative of FT-IR-ATR spectra, for compositional analyses of CS-HAp, were used. The SEM, MM, and AFM data have shown the formation of CS-HAp composite layers. The surface of CS-HAp composite layers showed uniform growth (at an Ar gas working pressure of p = 2 x 10(-3) mbar). The surface of the CS-HAp composites coatings became more nanostructured, becoming granular as the gas pressure increased from 5 x 10(-3) to 1.2 x 10(-2) mbar. However, our studies revealed that the surface morphology of the CS-HAp composite layers varies with the Ar gas working pressure. At the same time, optical properties are slightly influenced by Ar pressure. Their unique physicochemical properties make them suitable for various applications in the biomedical field, if we consider the already proven antimicrobial properties of chitosan. The antifungal properties and the capacity of the CS-HAp composite layers to inhibit the development of fungal biofilms were also demonstrated using the Candida albicans ATCC 10231 (C. albicans) fungal strain.

35. Multi-Level Evaluation of UV Action upon Vitamin D Enhanced, Silver Doped Hydroxyapatite Thin Films Deposited on Titanium Substrate

Authors: Negrila, CC; Predoi, D; Ghita, RV; Iconaru, SL; Ciobanu, SC; Manea, M; Badea, ML; Costescu, A; Trusca, R; Predoi, G; Stanciu, GA; Hristu, R; Dragu, LD; Bleotu, C; Groza, A; Marinas, IC; Chifiriuc, MC

Published: FEB 2021, COATINGS, 11, DOI: 10.3390/coatings11020120

Hydroxyapatite Ca-10(PO4)(6)(OH)(2) (HAp) is an important bioactive material for bone tissue reconstruction, due to its highly thermodynamic stability at a physiological pH without bio-resorption. In the present study, the Ag:HAp and the corresponding Ag:HAp + D-3 thin films (similar to 200 nm) coating were obtained by vacuum deposition method on Ti substrate. The obtained samples were exposed to different UV irradiation times, in order to investigate the UV light action upon thin films, before considering this method for the thin film's decontamination. The effects of UV irradiation upon Ag:Hap + D-3 are presented for the first time in the literature, marking a turning point for understanding the effect of UV light on composite biomaterial thin films. The UV irradiation induced an increase in the initial stages of surface roughness of Ag:HAp thin film, correlated with the modifications of XPS and FTIR signals. The characteristics of thin films measured by AFM (RMS) analysis corroborated with XPS and FTIR investigation highlighted a process of recovery of the thin film's properties (e.g., RMS), suggesting a possible adaptation to UV irradiation. This process has been a stage to a more complicated UVA rapid degradation process. The antifungal assays demonstrated that all the investigated samples exhibited antifungal properties. Moreover, the cytotoxicity assays revealed that the HeLa cells morphology did not show any alterations after 24 h of incubation with the Ag:HAp and Ag:HAp + D-3 thin films.

36. Nitrogen and Bromide Co-Doped Hydroxyapatite Thin Films with Antimicrobial Properties

Authors: Iconaru, SL; Ciobanu, CS; Predoi, D; Motelica-Heino, M; Negrila, CC; Badea, ML; Predoi, MV; Chifiriuc, CM; Popa, M

Published: DEC 2021, COATINGS, 11, DOI: 10.3390/coatings11121505

Hydroxyapatite (Ca-10(PO4)(6)(OH)(2), HAp), due to its high biocompatibility, is widely used as biomaterial. Doping with various ions of hydroxyapatite is performed to acquire properties as close as possible to the biological apatite present in bones and teeth. In this research the results of a study performed on thin films of hydroxyapatite co-doped with nitrogen and bromine (NBrHAp) are presented for the first time. The NBrHAp suspension was obtained by performing the adapted co-precipitation method using cetyltrimethylammonium bromide (CTAB). The thin layers of NBrHAp were obtained by spin-coating. The stability of the NBrHAp suspension was examined by ultrasound measurements. The thin layers obtained by the spin-coating method were examined by scanning electron microscopy (SEM), optical microscopy (OM), and metallographic microscopy (MM). The presence of nitrogen and bromine were highlighted by energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) studies. Fourier transform infrared spectroscopy (FTIR) was used to highlight the chemical status of nitrogen and bromine. In addition, the powder obtained from the NBrHAp suspension was analyzed by XRD. Moreover, the in vitro antimicrobial activity of the NBrHAp suspensions and coatings was investigated using the reference microbial strains Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231. The results highlighted the successful obtainment of N and Br co-doped hydroxyapatite suspension for the first time by an adapted co-precipitation method. The obtained suspension was used to produce pure NBrHAp composite thin films with superior morphological properties. The NBrHAp suspensions and coatings exhibited in vitro antimicrobial activity against bacterial and fungal strains and revealed their good antimicrobial activity.

37. Biocompatibility and Antibiofilm Properties of Samarium Doped Hydroxyapatite Coatings: An In Vitro Study

Authors: Nica, IC; Popa, M; Marutescu, L; Dinischiotu, A; Iconaru, SL; Ciobanu, SC; Predoi, D

Published: OCT 2021, COATINGS, 11, DOI: 10.3390/coatings11101185

The implant-related infection as a consequence of bacterial adherence and biofilm formation remains one of the main causes of implant failure. Grace to recent advances in materials science, their great mechanical properties and their biocompatibility (both in vitro and in vivo), antibacterial coatings have gradually become a primary component of the global strategy for preventing microbial colonization. In the present work, novel antibacterial coatings containing hydroxyapatite nanoparticles doped with two different concentrations of samarium (5SmHAp and 10SmHAp) were obtained on Si substrates using the dip coating method. The morphology and physicochemical properties of these modified surfaces were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). In addition, their antimicrobial effects and biocompatibility were assessed. The results showed a continuous and homogeneous layer, uniformly deposited, with no cracks or impurities. 5SmHAp and 10SmHAp surfaces exhibited significant antibiofilm activity and good biocompatibility without inducing cytotoxic effects in human gingival fibroblasts. All these findings indicate that samarium doped hydroxyapatite coatings could be great candidates for the development of new antimicrobial strategies.

38. Preparation and Characterization of Dextran Coated Iron Oxide Nanoparticles Thin Layers

Authors: Predoi, G; Ciobanu, CS; Iconaru, SL; Predoi, D; Dreghici, DB; Groza, A; Barbuceanu, F; Cimpeanu, C; Badea, ML; Barbuceanu, SF; Furnaris, CF; Belu, C; Ghegoiu, L; Raita, MS

Published: JUL 2021, POLYMERS, 13, DOI: 10.3390/polym13142351

In the present study, we report the synthesis of a dextran coated iron oxide nanoparticles (DIO-NPs) thin layer on glass substrate by an adapted method. The surface morphology of the obtained samples was analyzed by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), optical, and metallographic microscopies. In addition, the distribution of the chemical elements into the DIO-NPs thin layer was analyzed by Glow Discharge Optical Emission Spectrometry (GDOES). Furthermore, the chemical bonds formed between the dextran and iron oxide nanoparticles was investigated by Fourier Transform Infrared Spectroscopy (FTIR). Additionally, the HepG2 viability incubated with the DIO-NPs layers was evaluated at different time intervals using MTT (3-(4, 5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. The goal of this study was to obtain a DIO-NPs thin layer which could be used as a coating for medical devices such as microfluidic channel, microchips, and catheter. The results of the surface morphology investigations conducted on DIO-NPs thin layer suggests the presence of a continuous and homogeneous layer. In addition, the GDOES results indicate the presence of C, H, Fe, and O signal intensities characteristic to the DIO-NPs layers. The presence in the IR spectra of the Fe-CO metal carbonyl vibration bonds prove that the linkage between iron oxide nanoparticles and dextran take place through carbon-oxygen bonds. The cytotoxicity assays highlighted that HepG2 cells morphology did not show any noticeable modifications after being incubated with DIO-NPs layers. In addition, the MTT assay suggested that the DIO-NPs layers did not present any toxic effects towards HEpG2 cells.

39. The Physico-Chemical Properties and Exploratory Real-Time Cell Analysis of Hydroxyapatite Nanopowders Substituted with Ce, Mg, Sr, and Zn (0.5-5 at.%)

Authors: Chirica, IM; Enciu, AM; Tite, T; Dudau, M; Albulescu, L; Iconaru, SL; Predoi, D; Pasuk, I; Enculescu, M; Radu, C; Mihalcea, CG; Popa, AC; Rusu, N; Nita, S; Tanase, C; Stan, GE

Published: JUL 2021, MATERIALS, 14, DOI: 10.3390/ma14143808

Cation-substituted hydroxyapatite (HA), standalone or as a composite (blended with polymers or metals), is currently regarded as a noteworthy candidate material for bone repair/regeneration either in the form of powders, porous scaffolds or coatings for endo-osseous dental and orthopaedic implants. As a response to the numerous contradictions reported in literature, this work presents, in one study, the physico-chemical properties and the cytocompatibility response of single cation-doped (Ce, Mg, Sr or Zn) HA nanopowders in a wide concentration range (0.5-5 at.%). The modification of composition, morphology, and structure was multiparametrically monitored via energy dispersive X-ray, X-ray photoelectron, Fourier-transform infrared and micro-Raman spectroscopy methods, as well as by transmission electron microscopy and X-ray diffraction. From a compositional point of view, Ce and Sr were well-incorporated in HA, while slight and pronounced deviations were observed for Mg and Zn, respectively. The change of the lattice parameters, crystallite size, and substituting cation occupation factors either in the Ca(I) or Ca(II) sites were further determined. Sr produced the most important HA structural changes. The in vitro biological performance was evaluated by the (i) determination of leached therapeutic cations (by inductively coupled plasma mass spectrometry) and (ii) assessment of cell behaviour by both conventional assays (e.g., proliferation-3-(4,5-dimethyl thiazol-2-yl) 5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium assay; cytotoxicity-lactate dehydrogenase release assay) and, for the first time, real-time cell analysis (RTCA). Three cell lines were employed: fibroblast, osteoblast, and endothelial. When monophasic, the substituted HA supported the cells' viability and proliferation without signs of toxicity. The RTCA results indicate the excellent adherence of cells. The study strived to offer a perspective on the behaviour of Ce-, Mg-, Sr-, or Zn-substituted HAs and to deliver a well-encompassing viewpoint on their effects. This can be highly important for the future development of such bioceramics, paving the road toward the identification of candidates with highly promising therapeutic effects.

40. Development of Iron-Doped Hydroxyapatite Coatings

Authors: Predoi, D; Iconaru, SL; Ciobanu, SC; Predoi, SA; Buton, N; Megier, C; Beuran, M

Published: FEB 2021, COATINGS, 11, DOI: 10.3390/coatings11020186

It is known that iron is found as a trace element in bone tissue, the main inorganic constituent of which is hydroxyapatite. Therefore, iron-doped hydroxyapatite (HApFe) materials could be new alternatives for many biomedical applications. A facile dip coating process was used to elaborate the iron-doped hydroxyapatite (HApFe) nanocomposite coatings. The HApFe suspension used to prepare the coatings was achieved using a co-precipitation method, which was adapted in the laboratory. The quality of the HApFe suspension was assessed through dynamic light scattering (DLS), ultrasonic measurements, and zeta potential values. The hydroxyapatite XRD patterns were observed in the HApFe nanocomposite with no significant shifting of peak positions, thus suggesting that the incorporation of iron did not significantly modify the hydroxyapatite structure. The morphology of the HApFe nanoparticles was evaluated using transmission electron microscopy (TEM). Scanning electron microscopy (SEM) was used in order to investigate the morphologies of HApFe particles and coatings, while their chemical compositions were assessed using energy-dispersive X-ray spectroscopy (EDS). The SEM results suggested that the HApFe consists mainly of spherical nanometric particles and that the surfaces of the coatings are continuous and homogeneous. Additionally, the EDS spectra highlighted the purity of the samples and confirmed the presence of calcium, phosphorous, and iron in the analyzed sample. The in vitro cytotoxicity of the HApFe suspensions and coatings was evidenced using osteoblast cells. The MTT assay showed that both the HApFe suspensions and coatings exhibited biocompatible properties.

41. Removal and Oxidation of As(III) from Water Using Iron Oxide Coated CTAB as Adsorbent

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Motelica-Heino, M

Published: AUG 2020, POLYMERS, 12, DOI: 10.3390/polym12081687

Iron oxides such as magnetite and maghemite coated with cetyltrimethylammonium bromide (CTAB) are very promising materials for wastewater treatment because iron oxide can be easily separated from solutions using the magnetic separation procedure Iron oxide (IO) coated CTAB was synthesized by an adapted co-precipitation method. In the present study, the IO-CTAB was used for removing arsenic from water for the first time. In the present study, the performance of iron oxide coated CTAB biocomposites as an adsorbent for arsenic removal from aqueous solutions was examined. X-ray diffraction (XRD) analysis and the results revealed a cubic phase Fd-3 m of Fe(3)O(4)with lattice a = 8.40 angstrom and average crystal size equal to 17.26 +/- 3 nm. The mean particle size calculated from transmission electron microscopy (TEM) was 19.86 +/- 1.7 nm. The results of the adsorption batch experiments and the data determined using the Langmuir and Freundlich models emphasized that IO-CTAB nanoparticles were favorable for the adsorption of As(III) ions from aqueous solutions. Ultrasound measurements have shown that IO-CTAB is a cost-effective biocomposite for removing arsenic from contaminated solutions. Moreover, x-ray photoelectron spectroscopy (XPS) has shown that during the process of arsenic absorption, there is oxidation from As(III) to As(V), which leads to a decrease in toxicity during this process. The results of the cytotoxic assays confirmed that the IO-CTAB nanoparticles did not induce any morphological changes in the HeLa cells and did not affect their proliferation after 24 h of incubation.

42. Multifunctional Hydroxyapatite Coated with Arthemisia absinthium Composites

Authors: Raita, MS; Iconaru, SL; Groza, A; Cimpeanu, C; Predoi, G; Ghegoiu, L; Badea, ML; Chifiriuc, MC; Marutescu, L; Trusca, R; Furnaris, CF; Turculet, CS; Enache, DV; Predoi, D

Published: JAN 2 2020, MOLECULES, 25, DOI: 10.3390/molecules25020413

There is significant research showing that essential oils extracted from the plants have antibacterial effects. The purpose of this study was to develop a biocomposite based on hydroxyapatite coated with Artemisia absinthium essential oil and to highlight its antibacterial activity. Therefore, present studies are aimed at developing new materials combining hydroxyapatite with Artemisia absinthium essential oil, in order to avoid postoperative infections. The purpose of this work is to highlight the antimicrobial properties of the Artemisia absinthium essential oil-hydroxyapatite composites obtained by a simple method and at low costs. The structural properties and antimicrobial efficiency of the Artemisia absinthium essential oil-hydroxyapatite composite have been studied. The samples based on Artemisia absinthium essential oil analyzed in this study showed that wormwood essential oil presented the highest efficacy against the fungal strain of C. parapsilosis. It has been shown that wormwood essential oil has a strong antimicrobial effect against the microbial strains tested in this study. Furthermore, the antimicrobial properties of the biocomposites based on hydroxyapatite and essential oil are due to the presence of the essential oil in the samples.

43. Development of Cerium-Doped Hydroxyapatite Coatings with Antimicrobial Properties for Biomedical Applications

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Groza, A; Gaiaschi, S; Rokosz, K; Raaen, S; Negrila, CC; Prodan, AM; Costescu, A; Badea, ML; Chapon, P

Published: JUN 2020, COATINGS, 10, DOI: 10.3390/coatings10060516

Antibacterial cerium-doped hydroxyapatite (Ce-HAp) layers have been researched sparingly in recent years. The Ce-HAp powder, Ca10-xCex(PO4)(6)(OH()2)with x(Ce)= 0.05, was obtained by an adapted chemical co-precipitation method at room temperature. The target was prepared using the Ce-HAp (x(Ce)= 0.05) powder sintered in air at 600 degrees C. The coatings on the Ti substrate were generated in plasma using a radio frequency (RF) magnetron sputtering discharge in an Ar gas flow in a single run. To collect the most complete information regarding the antimicrobial activity of cerium-doped hydroxyapatite with x(Ce)= 0.05, (5Ce-HAp), antimicrobial studies were carried out both on the final suspensions and on the coated surfaces. The target was tested using ultrasound measurement, transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), glow-discharge optical emission spectroscopy (GDOES), and X-ray photoelectron spectroscopy (XPS). The present study exhibited for the first time results of the homogeneous coatings of hydroxyapatite doped with cerium using a radio frequency magnetron sputtering technique. In addition, this study highlighted for the first time the stability of the cerium-doped hydroxyapatite gels used in the creation of the coating. Ultrasound measurements on the concentrated suspension of 5Ce-HAp showed a good stability compared to double distilled, water which was chosen as the reference fluid. Particles with spherical shape were observed by both TEM and SEM analysis. The broadening of the IR bands in the IR spectrum of the 5Ce-HAp film in comparison with the IR spectrum of the precursor target indicate the formation of interlinked bonds into the layer bulk. XPS analysis revealed that the mixture of Ce(3+)and Ce(4+)ions in the hydroxyapatite (HAp) structure of the coatings could be due to the deposition process. The surface of 5Ce-HAp coatings was homogenous with particles having a spherical shape. A uniform distribution of all the constituent elements on the surface the 5Ce-HAp layer was revealed. The antimicrobial assays proved that both 5Ce-HAp suspensions and 5Ce-HAp coatings effectively inhibited the development of colony forming units (CFU) for all the tested microbial strains. Moreover, the antimicrobial assays emphasized that the 5Ce-HAp suspensions had a biocide effect against Escherichia coli (E. coli) andCandida albicans(C. albicans)microbial strains after 72 h of incubation.

44. Dextran-Thyme Magnesium-Doped Hydroxyapatite Composite Antimicrobial Coatings

Authors: Iconaru, SL; Predoi, MV; Motelica-Heino, M; Predoi, D; Buton, N; Megier, C; Stan, GE

Published: JAN 2020, COATINGS, 10, DOI: 10.3390/coatings10010057

The dextran-thyme magnesium-doped hydroxyapatite (10MgHAp-Dex-thyme) composite layers were prepared by a dip-coating procedure from stable suspensions and further analyzed for the first time. Different characterization techniques were employed to explore the physical-chemical features of the 10MgHAp-Dex-thyme suspensions and derived coatings. Information regarding the 10MgHAp-Dex-thyme suspensions was extracted on the basis of dynamic light scattering, zeta potential, and ultrasound measurements. The crystalline quality of the biocomposite powders-resulting after the centrifugation of suspensions-and the layers deposited on glass was assessed by X-ray diffraction in symmetric and grazing incidence geometries, respectively. The chemical structure and presence of functional groups were evaluated for both powder and coating by Fourier transform infrared spectroscopy in attenuated total reflectance mode. The extent of the antimicrobial effect range of the biocomposite suspensions and coatings was tested against different Gram-positive and Gram-negative bacteria (Staphylococcus aureus, Enterococcus faecalis, Escherichia coli, and Pseudomonas aeruginosa) and fungus (Candida albicans) strains with promising results.

45. Obtaining and Characterizing Thin Layers of Magnesium Doped Hydroxyapatite by Dip Coating Procedure

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Motelica-Heino, M; Buton, N; Megier, C

Published: JUN 2020, COATINGS, 10, DOI: 10.3390/coatings10060510

A simple dip coating procedure was used to prepare the magnesium doped hydroxyapatite coatings. An adapted co-precipitation method was used in order to obtain a Ca25-xMgx(PO4)(6)(OH)(2), 25MgHAp (x(Mg)= 0.25) suspension for preparing the coatings. The stabilities of 25MgHAp suspensions were evaluated using ultrasound measurements, zeta potential (ZP), and dynamic light scattering (DLS). Using transmission electron microscopy (TEM) and scanning electron microscopy (SEM) information at nanometric resolution regarding the shape and distribution of the 25MgHAp particles in suspension was obtained. The surfaces of obtained layers were evaluated using SEM and atomic force microscopy (AFM) analysis. The antimicrobial evaluation of 25MgHAp suspensions and coatings on various bacterial strains and fungus were realized. The present study presents important results regarding the physico-chemical and antimicrobial studies of the magnesium doped hydroxyapatite suspensions, as well as the coatings. The studies have shown that magnesium doped hydroxyapatite suspensions prepared withx(Mg)= 0.25 presented a good stability and relevant antimicrobial properties. The coatings made using 25MgHAp suspension were homogeneous and showed remarkable antimicrobial properties. Also, it was observed that the layer realized has antimicrobial properties very close to those of the suspension. Both samples of the 25MgHAp suspensions and coatings have very good biocompatible properties.

46. Antimicrobial Properties of Samarium Doped Hydroxyapatite Suspensions and Coatings

Authors: Iconaru, SL; Groza, A; Gaiaschi, S; Rokosz, K; Raaen, S; Ciobanu, SC; Chapon, P; Predoi, D

Published: NOV 2020, COATINGS, 10, DOI: 10.3390/coatings10111124

Post-implant infections are a major health problem, and it is well-known that treating them with conventional drugs is accompanied by many disadvantages. The development of new biomaterials with enhanced antimicrobial properties are of major interest for the scientific world. The aim of this study was to synthesize and characterize hydroxyapatite doped with Samarium (Ca10-xSmx(PO4)(6)(OH)(2), x(Sm) = 0.05, 5Sm-HAp) suspensions, pellets and coatings. The 5Sm-HAp coatings on Si substrates were obtained by rf magnetron sputtering technique. The different techniques such as ultrasound measurements, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Glow Discharge Optical Emission Spectroscopy (GDOES), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) were used to examine the obtained coatings. The results showed that the doped Sm ions entered the structure of hydroxyapatite successfully and Sm ions was uniformly doped onto the surface of the support. The depth profile curves of Ca, P, O, H, Ce and Si elements exhibit their presence from a surface to substrate interface as function of sputtering time. XPS analysis indicated as calcium-phosphate structures enriched in Sm3+ ions. Furthermore, the antimicrobial properties of the 5Sm-HAp suspensions, targets and coatings were assessed against Escherichia coli ATCC 25922, Staphylococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results of the antimicrobial assays highlighted that that the samples presented a strong antimicrobial activity against the tested microbial strains. The results showed that the coatings after 48 h of incubation inhibited the growth of all tested microbial strains under the value of 0.6 Log CFU/mL. This study shows that the 5Sm-HAp samples are good candidates for the development of new antimicrobial agents.

47. Physico-Chemical Properties and In Vitro Antifungal Evaluation of Samarium Doped Hydroxyapatite Coatings

Authors: Ciobanu, SC; Iconaru, SL; Predoi, D; Prodan, AM; Predoi, MV

Published: SEP 2020, COATINGS, 10, DOI: 10.3390/coatings10090827

Hydroxyapatite (HAp) and samarium doped hydroxyapatite, Ca10-xSmx(PO4)(6)(OH)(2),x(Sm)= 0.05, (5SmHAp), coatings were prepared by sol-gel process using the dip coating method. The stability of 5SmHAp suspension was evaluated by ultrasound measurements. Fourier transform infrared spectroscopy (FTIR) was used to examine the optical characteristics of HAp and 5SmHAp nanoparticles in suspension and coatings. The FTIR analysis revealed the presence of the functional groups specific to the structure of hydroxyapatite in the 5SmHAp suspensions and coatings. The morphology of 5SmHAp nanoparticles in suspension was evaluated by transmission electron microscopy (TEM). Moreover, scanning electron microscope (SEM) was used to evaluate the morphology of nanoparticle in suspension and the morphology of the surface on the coating. The SEM and TEM studies on 5SmHAp nanoparticles in suspension showed that our samples consist of nanometric particles with elongated morphology. The SEM micrographs of HAp and 5SmHAp coatings pointed out that the coatings are continuous and homogeneous. The surface morphology of the 5SmHAp coatings was also assessed by Atomic Force Microscopy (AFM) studies. The AFM results emphasized that the coatings presented the morphology of a uniformly deposited layer with no cracks and fissures. The crystal structure of 5SmHAp coating was characterized by X-ray diffraction (XRD). The surface composition of 5SmHAp coating was analyzed by X-ray photoelectron spectroscopy (XPS). The XRD and XPS analysis shown that the Sm(3+)ions have been incorporated into the 5SmHAp synthesized material. The antifungal properties of the 5SmHAp suspensions and coatings were studied usingCandida albicansATCC 10231 (C. albicans) fungal strains. The quantitative results of the antifungal assay showed that colony forming unity development was inhibited from the early phase of adherence in the case of both suspensions and coatings. Furthermore, the adhesion, cell proliferation and biofilm formation of theC. albicanswere also investigated by AFM, SEM and Confocal Laser Scanning Microscopy (CLSM) techniques. The results highlighted that theC. albicansadhesion and cell development was inhibited by the 5SmHAp coatings. Moreover, the data also revealed that the 5SmHAp coatings were effective in stopping the biofilm formation on their surface. The toxicity of the 5SmHap was also investigated in vitro using HeLa cell line.

48. Chitosan-Hydroxyapatite Composite Layers Generated in Radio Frequency Magnetron Sputtering Discharge: From Plasma to Structural and Morphological Analysis of Layers

Authors: Dreghici, DB; Butoi, B; Predoi, D; Iconaru, SL; Stoican, O; Groza, A

Published: DEC 2020, POLYMERS, 12, DOI: 10.3390/polym12123065

Chitosan-hydroxyapatite composite layers were deposited on Si substrates in radio frequency magnetron sputtering discharges. The plasma parameters calculated from the current-voltage radio frequency-compensated Langmuir probe characteristics indicate a huge difference between the electron temperature in the plasma and at the sample holder. These findings aid in the understanding of the coagulation pattern of hydroxyapatite-chitosan macromolecules on the substrate surface. An increase in the sizes of the spherical-shape grain-like structures formed on the coating surface with the plasma electron number density was observed. The link between the chemical composition of the chitosan-hydroxyapatite composite film and the species sputtered from the target or produced by excitation/ionization mechanisms in the plasma was determined on the basis of X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and residual gas mass spectrometry analysis.

49. Fabrication of Silver- and Zinc-Doped Hydroxyapatite Coatings for Enhancing Antimicrobial Effect

Authors: Predoi, D; Iconaru, SL; Predoi, MV

Published: SEP 2020, COATINGS, 10, DOI: 10.3390/coatings10090905

This study develops, for the first time, composite coatings based on silver and zinc doped hydroxyapatite in chitosan matrix (AgZnHApCs). The AgZnHApCs composite coatings were prepared by dip coating method. The hydroxyapatite (HAp), biocompatible material for regenerating and strengthening damaged bones were doped with silver and zinc ions and coated with chitosan in order to produce a uniform and homogenous coating with biocompatibility and antimicrobial properties. The stability of AgZnHApCs suspensions was evaluated by ultrasound measurements. The value of stability parameters of AgZnHApCs suspension is in good agreement with the value of bidistilled water used as reference fluid. Homogeneously dispersed solutions of AgZnHApCs were synthesized to endeavor to optimize the physico-chemical and biological characteristics of the coatings obtained at room temperature. The AgZnHApCs composite suspension and coatings were analyzed using various investigation techniques, such as X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenylte-2H-tetrazolium bromide) assay and antimicrobial studies. The optical spectroscopy, atomic force microscopy (AFM), metallographic examination and X-ray photoelectron spectroscopy (XPS) on AgZnHApCs composite coatings were also conducted. Cell culture and MTT assays demonstrate that AgZnHApCs composite suspension and coatings have no negative effect on the cell viability and proliferation. The cell morphology was not affected in presence of AgZnHApCs composite suspension and coatings. The antimicrobial assays conducted againstStaphylococcus aureusATCC 25923,Escherichia coliATCC 25922, andCandida albicansATCC 90029 microbial strains revealed that both the AgZnHApCs composite suspension and coatings exhibited great antimicrobial properties.

50. Silver-Doped Hydroxyapatite Thin Layers Obtained by Sol-Gel Spin Coating Procedure

Authors: Prodan, AM; Iconaru, SL; Predoi, MV; Predoi, D; Motelica-Heino, M; Turculet, CS; Beuran, M

Published: JAN 2020, COATINGS, 10, DOI: 10.3390/coatings10010014

The main objective of this paper is to develop silver-doped hydroxyapatite suspensions (HApAg) with different concentrations of silver (x(Ag) = 0.05 and x(Ag) = 0.2) in order to obtain uniform and homogenous layers by spin-coating procedure. The colloidal properties of HApAg suspensions are evaluated by dynamic light scattering (DLS) analysis, zeta-potential (ZP), and ultrasound measurements. The ultrasound studies show that the HApAg20 sample revealed better stability than the HApAg5 sample. The structural and morphological analysis on suspensions and thin layers is also conducted. It is observed that the particles of the two samples have a similar shape and are uniform. The layers obtained present a homogeneous appearance of the surface without evidence of cracks or interruption of the coatings. The in vitro antifungal studies conducted on the two thin layers at two different time intervals (24 and 48 h) show that both HApAg5 (x(Ag) = 0.05) and HApAg20 (x(Ag) = 0.05) nanoparticles suspensions and composite layers inhibit the development of colony forming units (CFU) even after 24 h of incubation comparative to the control, represented by the Candida albicans (C. albicans) culture in a proper medium. The fungicidal effect was evident after 48 h of incubation in the case of both HApAg20 nanoparticles suspensions and composite layers.

51. Peppermint Essential Oil-Doped Hydroxyapatite Nanoparticles with Antimicrobial Properties

Authors: Badea, ML; Iconaru, SL; Groza, A; Chifiriuc, MC; Beuran, M; Predoi, D

Published: JUN 1 2019, MOLECULES, 24, DOI: 10.3390/molecules24112169

This study aimed at developing an antimicrobial material based on hydroxyapatite (HAp) and peppermint essential oil (P-EO) in order to stimulate the antimicrobial activity of hydroxyapatite. The molecular spectral features and morphology of the P-EO, HAp and hydroxyapatite coated with peppermint essential oil (HAp-P) were analyzed using Fourier-transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The coating of the HAp with the P-EO did not affect the ellipsoidal shape of the nanoparticles. The overlapping of IR bands of P-EO and HAp in the HAp-P spectrum determined the formation of the broad molecular bands that were observed in the spectral regions of 400-1000 cm(-1) and 1000-1200 cm(-1). The antibacterial activity of the P-EO, HAp and HAp-P were also tested against different Gram-positive bacteria (methicillin-resistant Staphylococcus aureus (MRSA) 388, S. aureus ATCC 25923, S. aureus ATCC 6538, E. faecium DSM 13590), Gram-negative bacteria (Escherichia coli ATCC 25922, E. coli C5, P. aeruginosa ATCC 27853, P. aeruginosa ATCC 9027) and a fungal strain of Candida parapsilosis. The results of the present study revealed that the antimicrobial activity of HAp-P increased significantly over that of HAp.

52. The Effect of the Ionizing Radiation on Hydroxyapatite-Polydimethylsiloxane Layers

Authors: Groza, A; Iconaru, SL; Jiga, G; Chapon, P; Gaiaschi, S; Verga, N; Beuran, M; Prodan, AM; Matei, M; Marinescu, SA; Trusca, R; Predoi, D

Published: DEC 2019, POLYMER ENGINEERING AND SCIENCE, 59, 2412, DOI: 10.1002/pen.25247

The bio hydroxyapatite (HAp) was used from a long time in different medical and environmental applications. The HAp layers with a uniform surface were used for various medical applications such as orthopedic and dental metal implants. In this work, we reported on the influence of X-ray radiation on the structural and morphological properties of composite layers based on HAp and polydimethylsiloxane (PDMS) deposited on titanium substrates. The HAp:PDMS layers were investigated by different complementary methods such as scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and glow discharge optical emission spectrometry (GDOES). FTIR spectral analysis showed that the molecular structure of the coatings was not changed after their irradiation even though, the depth profile analysis performed by GDOES indicated a depletion of Ca and P elements from the HAp:PDMS irradiated samples. By SEM, we showed that the morphological features of the coatings were also changed, as the irradiated layers are delaminated. The biological assays confirmed that the antibacterial activity of HAp:PDMS composite layers increased after irradiation. The results obtained in this study highlighted that the biological properties of HAp:PDMS layers could be influenced by irradiation. (C) 2019 Society of Plastics Engineers.

53. Preparations of Silver/Montmorillonite Biocomposite Multilayers and Their Antifungal Activity

Authors: Iconaru, SL; Groza, A; Stan, GE; Predoi, D; Gaiaschi, S; Trusca, R; Chifiriuc, CM; Marutescu, L; Tite, T; Stanciu, GA; Hristu, R; Ghegoiu, L; Badea, ML; Turculet, CS; Ganciu, M; Chapon, P

Published: DEC 2019, COATINGS, 9, DOI: 10.3390/coatings9120817

In this study, the results about the influence of the surface morphology of layers based on montmorillonite (MMT) and silver (Ag) on antimicrobial properties are reported. The coating depositions were performed in the plasma of a radio frequency (RF) magnetron sputtering discharge. The studied layers were single montmorillonite layers (MMT) and silver/montmorillonite multilayers (MMT-Ag) obtained by magnetron sputtering technique with a different surface thickness. The resultant MMT-Ag biocomposite multilayers exhibited a uniform distribution of constituent elements and enhanced antimicrobial properties against fungal biofilm development. Glow-discharge optical emission spectroscopy (GDOES) analysis revealed the formation of MMT-Ag biocomposite multilayers following the deposit of a silver layer for an MMT layer that was initially deposited on a Si substrate. The surface morphology and thickness evaluation of deposited biocomposite layers were performed by scanning electron microscopy (SEM). A qualitative analysis of the chemical composition of thin layers was performed and the elements O, Ag, Mg, Fe, Al, and Si were identified in the MMT-Ag biocomposite multilayers. The in vitro antifungal assay proved that the inhibitory effect against the growth of Candida albicans ATCC 101231 CFU was more emphasized in the case of MMT-Ag biocomposite multilayers that in the case of the MMT layer. Cytotoxicity studies performed on HeLa cells showed that the tested layers did not show significant toxicity at the time intervals during which the assay was performed. On the other hand, it was observed that the MMT layers exhibited slightly higher biocompatible properties than the MMT-Ag composite layers.

54. Biocompatible Layers Obtained from Functionalized Iron Oxide Nanoparticles in Suspension

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Buton, N; Megier, C; Motelica-Heino, M

Published: DEC 2019, COATINGS, 9, DOI: 10.3390/coatings9120773

Iron oxide nanoparticles have been extensively studied for challenges in applicable areas such as medicine, pharmacy, and the environment. The functionalization of iron oxide nanoparticles with dextran opens new prospects for application. Suspension characterization methods such as dynamic light scattering (DLS) and zeta potential (ZP) have allowed us to obtain information regarding the stability and hydrodynamic diameter of these suspended particles. For rigorous characterization of the suspension of dextran-coated iron oxide nanoparticles (D-MNPs), studies have been performed using ultrasound measurements. The results obtained from DLS and ZP studies were compared with those obtained from ultrasound measurements. The obtained results show a good stability of D-MNPs. A comparison between the D-MNP dimension obtained from transmission electron microscopy (TEM), X-ray diffraction (XRD), and DLS studies was also performed. A scanning electron spectroscopy (SEM) image of a surface D-MNP layer obtained from the stable suspension shows that the particles are spherical in shape. The topographies of the elemental maps of the D-MNP layer showed a uniform distribution of the constituent elements. The homogeneity of the layer was also observed. The morphology of the HeLa cells incubated for 24 and 48 h with the D-MNP suspension and D-MNP layers did not change relative to the morphology presented by the control cells. The cytotoxicity studies conducted at different time intervals have shown that a slight decrease in the HeLa cell viability after 48 h of incubation for both samples was observed.

55. Photoluminescent Hydroxylapatite: Eu3+ Doping Effect on Biological Behaviour

Authors: Andronescu, E; Predoi, D; Neacsu, IA; Paduraru, AV; Musuc, AM; Trusca, R; Oprea, O; Tanasa, E; Vasile, OR; Nicoara, AI; Surdu, AV; Iordache, F; Birca, AC; Iconaru, SL; Vasile, BS

Published: SEP 2019, NANOMATERIALS, 9, DOI: 10.3390/nano9091187

Luminescent europium-doped hydroxylapatite (Eu(X)HAp) nanomaterials were successfully obtained by co-precipitation method at low temperature. The morphological, structural and optical properties were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), UV-Vis and photoluminescence (PL) spectroscopy. The cytotoxicity and biocompatibility of Eu(X)HAp were also evaluated using MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide)) assay, oxidative stress assessment and fluorescent microscopy. The results reveal that the Eu3+ has successfully doped the hexagonal lattice of hydroxylapatite. By enhancing the optical features, these Eu(X)HAp materials demonstrated superior efficiency to become fluorescent labelling materials for bioimaging applications.

56. Synthesis, Characterization, and Antimicrobial Activity of Magnesium-Doped Hydroxyapatite Suspensions

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Stan, GE; Buton, N

Published: SEP 2019, NANOMATERIALS, 9, DOI: 10.3390/nano9091295

Obtaining nanoscale materials has allowed for the miniaturization of components, which has led to the possibility of achieving more efficient devices with faster functions and much lower costs. While hydroxyapatite [HAp, Ca-10(PO4)(6)(OH)(2)] is considered the most widely used material for medical applications in orthopedics, dentistry, and general surgery, the magnesium (Mg) is viewed as a promising biodegradable and biocompatible implant material. Furthermore, Mg is regarded as a strong candidate for developing medical implants due to its biocompatibility and antimicrobial properties against gram-positive and gram-negative bacteria. For this study, magnesium-doped hydroxyapatite (Ca10-xMgx (PO4)(6) (OH)(2), x(Mg) = 0.1), 10MgHAp, suspensions were successfully obtained by an adapted and simple chemical co-precipitation method. The information regarding the stability of the nanosized 10MgHAp particles suspension obtained by zeta-potential analysis were confirmed for the first time by a non-destructive ultrasound-based technique. Structural and morphological studies of synthesized 10MgHAp were conducted by X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy in attenuated total reflectance (ATR) mode and scanning electron microscopy (SEM). The XRD analysis of the 10MgHAp samples confirmed that a single crystalline phase associated to HAp with an average grain size about 93.3 nm was obtained. The FTIR-ATR spectra revealed that the 10MgHAp sample presented broader IR bands with less visible peaks when compared to a well-crystallized pure HAp. The SEM results evidenced uniform MgHAp nanoparticles with spherical shape. The antimicrobial activity of the 10MgHAp suspension against gram-positive strains (Staphylococcus aureus ATCC 25923, Enterococcus faecalis ATCC 29212), gram-negative strains (Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853), as well as a fungal strain (Candida albicans ATCC 90029) were evaluated.

57. Zinc Doped Hydroxyapatite Thin Films Prepared by Sol-Gel Spin Coating Procedure

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Buton, N; Motelica-Heino, M

Published: FEB 28 2019, COATINGS, 9, DOI: 10.3390/coatings9030156

In this study, ZnHAp layers deposited on a Si substrate were obtained by a sol-gel spin-coating procedure. The ZnHAp solutions used to obtain the ZnHAp coatings were investigated by dynamic light scattering (DLS) analysis, zeta-potential, ultrasound measurements, and flame atomic absorption spectrometry (AAS). The average measured hydrodynamic diameter from the DLS analysis, zeta-potential, and ultrasound measurements were analyzed so as to characterize and estimate the stability of the ZnHAp nanoparticles. The AAS results confirmed the presence of zinc in the gels used in the preparation of the ZnHAp layers. The layers were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD results revealed the diffraction peaks of the hexagonal hydroxyapatite in all of the investigated samples. The morphology of the ZnHAp coatings annealed at 500 degrees C (ZnHAp-500) and 700 degrees C (ZnHAp-700), which evidenced that no fissures or cracks formed on the surface of the coatings. The biocompatibility assays indicated that the ZnHAp coatings did not present any toxicity towards the HeLa cells. Furthermore, the study regarding the cytotoxicity of the ZnHAp layers against microorganisms emphasized that ZnHAp coatings exhibited an inhibitory effect towards S. aureus bacterial cells and also towards C. albicans fungal cells.

58. Evaluation of Antibacterial Activity of Zinc-Doped Hydroxyapatite Colloids and Dispersion Stability Using Ultrasounds

Authors: Predoi, D; Iconaru, SL; Predoi, MV; Motelica-Heino, M; Guegan, R; Buton, N

Published: APR 2019, NANOMATERIALS, 9, DOI: 10.3390/nano9040515

This study proves that the new developed zinc-doped hydroxyapatite (ZnHAp) colloids by an adapted sol-gel method can be widely used in the pharmaceutical, medical, and environmental industries. ZnHAp nanoparticles were stabilized in an aqueous solution, and their colloidal dispersions have been characterized by different techniques. Scanning Electron Microscopy (SEM) was used to get information on the morphology and composition of the investigated samples. Energy-dispersive X-ray spectroscopy (EDX) analysis confirmed the elemental compositions of ZnHAp colloidal dispersions. The homogeneous and uniform distribution of constituent elements (zinc, calcium, phosphorus, oxygen) was highlighted by the obtained elemental mapping results. The X-ray diffraction (XRD) results of the obtained samples showed a single phase corresponding to the hexagonal hydroxyapatite. The characteristic bands of the hydroxyapatite structure were also evidenced by Fourier-transform infrared spectroscopy (FTIR) analysis. For a stability assessment of the colloidal system, -potential for the ZnHAp dispersions was estimated. Dynamic light scattering (DLS) was used to determine particles dispersion and hydrodynamic diameter (D-HYD). The goal of this study was to provide for the first time information on the stability of ZnHAp particles in solutions evaluated by non-destructive ultrasound-based technique. In this work, the influence of the ZnHAp colloidal solutions stability on the development of bacteria, such as Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus), was also established for the first time. The antimicrobial activity of ZnHAp solutions was strongly influenced by both the stability of the solutions and the amount of Zn.

59. Dextran-Coated Zinc-Doped Hydroxyapatite for Biomedical Applications

Authors: Predoi, D; Iconaru, SL; Predoi, MV

Published: MAY 2019, POLYMERS, 11, DOI: 10.3390/polym11050886

Dextran-coated zinc-doped hydroxyapatite (ZnHApD) was synthesized by an adapted sol-gel method. The stability of ZnHApD nanoparticles in an aqueous solution was analyzed using ultrasonic measurements. The analysis of the evolution in time of the attenuation for each of the frequencies was performed. The X-ray diffraction (XRD) investigations exhibited that no impurity was found. The morphology, size and size distribution of the ZnHApD sample was investigated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The TEM and SEM results showed that the ZnHApD particles have an ellipsoidal shape and a narrow distribution of sizes. The cell growth and toxicity of HEK-293 cells were investigated on the ZnHApD solution for four different concentrations and analyzed after 24 and 48 h. The ZnHApD solution presented a non-toxic activity against HEK-293 cells for all analyzed concentrations. The antibacterial assay revealed that all the tested microorganisms were inhibited by the ZnHApD dispersion after 24 and 48 h of incubation. It was observed that the effect of the ZnHApD solution on bacteria growth depended on the bacterial strain. The Porphyromonas gingivalis ATCC 33277 bacterial strain was the most sensitive, as a growth inhibition in the presence of 0.075 mu g/mL ZnHApD in the culture medium was observed.

60. Commercial Hydroxyapatite Powders for Lead Removal from Aqueous Solution

Authors: Negrila, CC; Iconaru, SL; Motelica-Heino, M; Guegan, R; Predoi, G; Barbuceanu, F; Ghita, RV; Petre, CC; Jiga, G; Badea, ML; Prodan, AM; Predoi, D

Published: 2018, 9TH INTERNATIONAL CONFERENCE ON TIMES OF POLYMERS AND COMPOSITES: FROM AEROSPACE TO NANOTECHNOLOGY, 1981, DOI: 10.1063/1.5045983

Nowadays, the advances materials science have created the possibility of using nanomaterials as adsorbents in environmental technologies. This study is focused on the evaluation of C-HAp powders capacity in lead ions removal from contaminated solutions. The C-HAp powders after removal of lead (Pb2+) ions from contaminated water were characterized by X-Ray Photoelectron Spectroscopy (XPS) and Energy Dispersive X-ray analysis (EDX). The presence of lead in the hydroxyapatite powders after removal experiments was observed in the XPS general spectrum and also in the EDX spectra. In addition, the AAS studies revealed that the C-HAp powders possess a high affinity towards lead ions with an effective removal rate of 80% for an initial lead concentration of 20 mg.L-1.

61. Antimicrobial Studies on Iron Oxide-Dextran Colloidal Suspension

Authors: Predoi, D; Iconaru, SL; Buton, N; Predoi, G; Barbuceanu, F; Petre, CC; Jiga, G; Badea, ML; Prodan, AM

Published: 2018, 9TH INTERNATIONAL CONFERENCE ON TIMES OF POLYMERS AND COMPOSITES: FROM AEROSPACE TO NANOTECHNOLOGY, 1981, DOI: 10.1063/1.5045967

Iron oxide-dextran nanoparticle suspensions (IOD-NPsS) have attracted attention for their considerable applications in various biomedical area such as cosmetics, water remediation, hyperthermia, drug delivery or magnetic resonance imaging (MRI) contrast enhancement. In these research we report the antimicrobial studies on iron oxide-dextran colloidal suspension against prokaryotic cells such as Escherichia coli (E. coli). The ultrasound studies and dynamic light scattering (DLS) of iron oxide-dextran nanoparticle suspensions. According colloidal studies of the iron oxide suspension, the nanoparticles was in dispersed state.

62. Physico-Chemical Characteristics and Antimicrobial Studies of Silver Doped Hydroxyapatite

Authors: Predoi, D; Predoi, MV; El Kettani, MEC; Leduc, D; Iconaru, SL; Ciobanu, CS; Buton, N; Petre, CC; Prodan, AM

Published: 2018, 7TH INTERNATIONAL CONFERENCE ON STRUCTURAL ANALYSIS OF ADVANCED MATERIALS (ICSAAM 2017), 1932, DOI: 10.1063/1.5024184

The present research is focused on the synthesis, structural and morphological characterization and antimicrobial evaluation of silver doped hydroxyapatite (AgHAp) in water. The preliminary ultrasonic characterizations of the AgHAp in water synthesized by an adapted co-precipitation method are also presented. X-ray diffraction result showed that silver ions were substituted in the hydroxyapatite structure. The lattice parameters increased when the silver substitution increased. The morphology of AgHAp were evaluated by Scanning Electron Microscopy (SEM). By EDX analysis the constituents elements of hydroxyapatite were detected in all analyzed samples. The silver was also found in the samples with x(Ag) = 0.5 and 0.2. The colloidal properties of the resulted AgHAp (x(Ag) = 0.0, 0.05 and 0.2) in water were analyzed by Dynamic Light Scattering (DLS) and zeta potential. On the other hand, the novelty of our research consists of preliminary ultrasonic measurements (US) conducted on AgHAp in water. Furthermore, the antimicrobial activity of AgHAp was evaluated and a decrease in the number of surviving cells was established.

63. Properties of Basil and Lavender Essential Oils Adsorbed on the Surface of Hydroxyapatite

Authors: Predoi, D; Groza, A; Iconaru, SL; Predoi, G; Barbuceanu, F; Guegan, R; Motelica-Heino, MS; Cimpeanu, C

Published: MAY 2018, MATERIALS, 11, DOI: 10.3390/ma11050652

The research conducted in this study presented for the first time results of physico-chemical properties and in vitro antimicrobial activity of hydroxyapatite plant essential oil against Gram-positive bacteria (methicillin-resistant Staphylococcus aureus (MRSA) and S. aureus 0364) and Gram-negative bacteria (Escherichia coli ATCC 25922). The samples were studied by scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy to determine the morphology and structure of the nanocomposites of hydroxyapatite coated with basil (HAp-B) and lavender (HAp-L) essential oils (EOs). The values of the BET specific surface area (S-BET), total pore volume (V-P) and pore size (D-P) were determined. The results for the physico-chemical properties of HAp-L and HAp-B revealed that lavender EOs were well adsorbed on the surface of hydroxyapatite, whereas basil EOs showed a poor adsorption on the surface of hydroxyapatite. We found that the lavender EOs hydroxyapatite (HAp-L) exhibited a very good inhibitory growth activity. The value of the minimum inhibitory concentration (MIC) related to growth bacteria was 0.039 mg/mL for MRSA, 0.02 mg/mL for S. aureus and 0.039 mg/mL E. coli ATCC 25922. The basil EO hydroxyapatite (HAp-B) showed poor inhibition of bacterial cell growth. The MIC value was 0.625 mg/mL for the HAp-B sample in the presence of the MRSA bacteria, 0.313 mg/mL in the presence of S. aureus and 0.078 mg/mL for E. coli ATCC 25922.

64. Bioceramic Layers with Antifungal Properties

Authors: Predoi, D; Iconaru, SL; Predoi, MV

Published: AUG 2018, COATINGS, 8, DOI: 10.3390/coatings8080276

The sol-gel method was used to synthesize the silver doped hydroxyapatite (Ag:HAp) gels in order to produce the antifungal composite layers. The pure Ti disks were used as the substrate for the composite layers. Important information about suspensions used to make Ag:HAp composite layers were obtained from an ultrasonic technique. The identification of the phase composition of the Ag:HAp composite layers was accomplished X-ray diffraction (XRD). The morphology and the thickness of the layers was evaluated using scanning electron microscopy (SEM). The uniform distribution of the constituent elements (Ag, Ca, P, and O) in both analyzed samples was observed. The antifungal activity of the samples against Candida albicans ATCC 10231 microbial strain were investigated immediately after their preparation and six months later. SEM and confocal laser scanning microscopy (CLSM) images showed that the composite layers at the two time intervals exhibited a strong antifungal activity against Candida albicans ATCC 10231 and completely inhibited the biofilm formation.

65. Fabrication and Characterization of Iron Oxide Dextran Composite Layers

Authors: Iconaru, SL; Predoi, SA; Beuran, M; Ciobanu, CS; Trusca, R; Ghita, R; Negoi, I; Teleanu, G; Turculet, SC; Matei, M; Badea, M; Prodan, AM

Published: 2018, 7TH INTERNATIONAL CONFERENCE ON STRUCTURAL ANALYSIS OF ADVANCED MATERIALS (ICSAAM 2017), 1932, DOI: 10.1063/1.5024169

Super paramagnetic iron oxide nanoparticles such as maghemite have been shown to exhibit antimicrobial properties [1-5]. Moreover, the iron oxide nanoparticles have been proposed as a potential magnetically controllable antimicrobial agent which could be directed to a specific infection [3-5]. The present research has focused on studies of the surface and structure of iron oxide dextran (D-IO) composite layers surface and structure. These composite layers were deposited on Si substrates. The structure of iron oxide dextran composite layers was investigated by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) while the surface morphology was evaluated by Scanning Electron Microscopy (SEM). The structural characterizations of the iron oxide dextran composite layers revealed the basic constituents of both iron and dextran structure. Furthermore, the in vitro evaluation of the antifungal effect of the complex layers, which have been shown revealed to be active against C. albicans cells at distinct intervals of time, is exhibited. Our research came to confirm the fungicidal effect of iron oxide dextran composite layers. Also, our results suggest that iron oxide dextran surface may be used for medical treatment of biofilm associated Candida infections.

66. Removal of Zinc Ions Using Hydroxyapatite and Study of Ultrasound Behavior of Aqueous Media

Authors: Iconaru, SL; Motelica-Heino, M; Guegan, R; Predoi, MV; Prodan, AM; Predoi, D

Published: AUG 2018, MATERIALS, 11, DOI: 10.3390/ma11081350

The present study demonstrates the effectiveness of hydroxyapatite nanopowders in the adsorption of zinc in aqueous solutions. The synthesized hydroxyapatites before (HAp) and after the adsorption of zinc (at a concentration of 50 mg/L) in solution (HApD) were characterized using X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM, respectively). The effectiveness of hydroxyapatite nanopowders in the adsorption of zinc in aqueous solutions was stressed out through ultrasonic measurements. Both Langmuir and Freundlich models properly fitted on a wide range of concentration the equilibrium adsorption isotherms, allowing us to precisely quantify the affinity of zinc to hydroxyapatite nanopowders and to probe the efficacy of hydroxyapatite in removal of zinc ions from aqueous solutions in ultrasonic conditions.

67. Influence of Ionizing Radiations on Structural and Antibacterial Properties of Hydroxyapatite-Polydimethylsiloxane Layers

Authors: Groza, A; Iconaru, SL; Petre, CC; Jiga, G; Badea, ML; Prodan, AM; Beuran, M; Chapon, P; Gaianschi, S; Ganciu, M; Verga, N; Trusca, R; Vineticu, N; Predoi, D

Published: 2018, 9TH INTERNATIONAL CONFERENCE ON TIMES OF POLYMERS AND COMPOSITES: FROM AEROSPACE TO NANOTECHNOLOGY, 1981, DOI: 10.1063/1.5045985

In the recent years a special attention has been granted to the generation and characterization of hydroxyapatite-polydimethylsiloxane layers especially due to their biomedical applications. In this context, in this paper, we analyzed the influence of X ray radiation delivered in medical dose on the morphological mid chemical structure of hydroxyapatite-polydimethylsiloxane layers deposited on Ti substrates. The damage effects produced by the ionizing radiation on the surface and structure of hydroxyapatite-polydimethylsiloxane layers were identified by Scanning Electron Microscopy (SEM) and Glow Discharge Optical Emission Spectroscopy (GDOES). The antibacterial activity of the irradiated and non irradiated samples was also evaluated.

68. Application of Biocompatible Magnetite Nanoparticles for the Removal of Arsenic and Copper from Water

Authors: Iconaru, SL; Beuran, M; Turculet, CS; Negoi, I; Teleanu, G; Prodan, AM; Motelica-Heino, M; Guegan, R; Ciobanu, CS; Jiga, G; Predoi, D

Published: 2018, 7TH INTERNATIONAL CONFERENCE ON STRUCTURAL ANALYSIS OF ADVANCED MATERIALS (ICSAAM 2017), 1932, DOI: 10.1063/1.5024168

The progress of nanotechnology made possible the use of nanomaterials as adsorbents and magnetic iron oxides represents one of the first generations of nanoscale materials used in environment technologies [1]. A systematic characterization of commercial magnetite (Fe3O4) is presented in this research. The commercial (Fe3O4) magnetic adsorbents were characterized by various characterizations methods such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray analysis (EDX). This study was also focused on the study of adsorption isotherms and the kinetics evaluation. X-ray studies indicated that As3+ and Cu2+ removed by Fe3O4 did not seem to alter the structure of Fe3O4 but they were highlighted in the EDX analysis. In addition, the SEM studies were consistent with the XRD results. The rate of adsorption of contaminants, in contaminated solutions decreases when the amount of contaminant increases in all experiments performed. The results revealed that Fe3O4 nanoparticles are promising candidates which could be used as sorbents for the removal of arsenic from the marine environment, for site remediation and groundwater treatment.

69. Adsorption of Pb (II) Ions onto Hydroxyapatite Nanopowders in Aqueous Solutions

Authors: Iconaru, SL; Motelica-Heino, M; Guegan, R; Beuran, M; Costescu, A; Predoi, D

Published: NOV 2018, MATERIALS, 11, DOI: 10.3390/ma11112204

Contamination of water with heavy metals such as lead is a major worldwide problem because they affect the physiological functions of living organisms, cause cancer, and damage the immune system. Hydroxyapatite, (Ca-5(PO4)(3)OH) is considered one of the most effective materials for removing heavy metals from contaminated water. The hydroxyapatite nanopowders (N-HAp) obtained by a co-precipitation method were used in this research to determine the effectiveness in removing lead ions from contaminated solutions. In this study, we have investigated the structure and morphology of N-HAp nanopowders using X-ray diffraction (XRD), electronic transmission microscopy (TEM), and scanning electron microscopy (SEM). The structure information was also obtained by spectroscopy measurements. The Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy measurements revealed the presence of peaks corresponding to the phosphate and hydroxyl groups. The ability of N-HAp nanopowders to adsorb lead ions from aqueous solutions were established. The results of the kinetic and equilibrium studies on the removal of Pb (II) from aqueous solution revealed that the adsorption of lead (II) cations is due to the surface reaction with the hydroxyl terminal groups on the adsorbent and the combination of the positive charges of the metal cations with the negative charges on the adsorbent surfaces. These observations could validate the use of these ceramic nanopowders in ecological remediation strategies.

70. Antimicrobial Activity of New Materials Based on Lavender and Basil Essential Oils and Hydroxyapatite

Authors: Predoi, D; Iconaru, SL; Buton, N; Badea, ML; Marutescu, L

Published: MAY 2018, NANOMATERIALS, 8, DOI: 10.3390/nano8050291

This study presents, for the first-time, the results of a study on the hydrodynamic diameter of essential oils (EOs) of basil and lavender in water, and solutions of EOs of basil (B) and lavender (L) and hydroxyapatite (HAp). The possible influence of basil and lavender EOs on the size of hydroxyapatite nanoparticles was analyzed by Scanning Electron Microscopy (SEM). We also investigated the in vitro antimicrobial activity of plant EOs and plant EOs hydroxyapatite respectively, against Gram-positive bacteria (methicillin-resistant Staphylococcus aureus1144 (MRSA 1144) and S. aureus 1426) and Gram-negative bacteria (Escherichia coli ATCC 25922 and Escherichia coli ESBL 4493). From the autocorrelation function, obtained by Dynamic Light Scattering (DLS) measurements it was observed that basil yielded one peak at an average hydrodynamic diameter of 354.16 nm, while lavender yielded one peak at an average hydrodynamic diameter of 259.76 nm. In the case of HAp nanoparticles coated with basil (HApB) and lavender (HApL) essential oil, the aggregation was minimal. We found that the lavender EO exhibited a very good inhibitory growth activity (MIC values ranging from <0.1% for E. coli reference strain to 0.78% for S. aureus strains). The biological studies indicated that HapL material displayed an enhanced antimicrobial activity, indicating the potential use of HAp as vehicle for low concentrations of lavender EO with antibacterial properties. Flow cytometry analysis (FCM) allowed us to determine some of the potential mechanisms of the antimicrobial activities of EOs, suggesting that lavender EO was active against E. coli by interfering with membrane potential, the membrane depolarization effect being increased by incorporation of the EOs into the microporous structure of HAp. These findings could contribute to the development of new antimicrobial agents that are urgently needed for combating the antibiotic resistance phenomena.

71. Development of Zinc-Doped Hydroxyapatite by Sol-Gel Method for Medical Applications

Authors: Negrila, CC; Predoi, MV; Iconaru, SL; Predoi, D

Published: NOV 2018, MOLECULES, 23, DOI: 10.3390/molecules23112986

Zinc- (Zn) doped hydroxyapatite (HAp) were prepared by sol-gel method. Zinc-doped hydroxyapatite (ZnHAp) and HAp were analyzed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The Rietveld analysis revealed that the HAp and 7ZnHAp powders obtained by sol-gel method have a monophasic hydroxyapatite structure belonging to the P6(3/m) spatial group. The results obtained from the ultrasound characterization of HAp and ZnHAp are also presented in this study. The effect of zinc concentration on properties that were deduced from ultrasonic measurements are studied in the case of a significant zinc concentration (x(Zn) = 0.07). From the values of the ultrasonic waves velocities were determined by the pairs of elastic coefficients of the suspensions (Young modulus E, Poisson coefficient nu), which have proven to be similar to those determined by other authors.

72. ZnHAp Thin Films for Medical Applications

Authors: Iconaru, SL; Groza, A; Chapon, P; Gaianschi, S; Petre, CC; Jiga, G; Beuran, M; Prodan, AM; Lupescu, O; Trusca, R; Predoi, D

Published: 2018, 9TH INTERNATIONAL CONFERENCE ON TIMES OF POLYMERS AND COMPOSITES: FROM AEROSPACE TO NANOTECHNOLOGY, 1981, DOI: 10.1063/1.5045984

The research regarding the properties of thin films of hydroxyapatite doped with various ions such as zinc elaborated by spin-coating technique have rarely been fabricated and studies in recent years. In the present study Zn doped hydroxyapatite (ZrHAp) synthesized by a sol-gel method were coated on Ti substrates using a spin-coating technique. The thin films was characterized by Scanning Electron Microscopy (SEM) and Glow Discharge Optical Emission Spectroscopy (GDOES). The structural characterizations of ZnHAp thin films showed the presence of Zn and apatitic structure. The GD depth profiles revealed the successful embedding of the Zn ions in HAp structure. In addition, in vitro evaluation of the antifungal properties of ZnHAp demonstrated the potential antifungal effect of ZnHAp thin films against Staphylococcus aureus 0364 biofilm.

73. Structural Characterization and Antifungal Studies of Zinc-Doped Hydroxyapatite Coatings

Authors: Iconaru, SL; Prodan, AM; Buton, N; Predoi, D

Published: APR 2017, MOLECULES, 22, DOI: 10.3390/molecules22040604

The present study is focused on the synthesis, characterization and antifungal evaluation of zinc-doped hydroxyapatite (Zn:HAp) coatings. The Zn:HAp coatings were deposited on a pure Si (Zn:HAp_Si) and Ti (Zn:HAp_Ti) substrate by a sol-gel dip coating method using a zinc-doped hydroxyapatite nanogel. The nature of the crystal phase was determined by X-ray diffraction (XRD). The crystalline phase of the prepared Zn:HAp composite was assigned to hexagonal hydroxyapatite in the P6(3/m) space group. The colloidal properties of the resulting Zn:HAp (x(Zn) = 0.1) nanogel were analyzed by Dynamic Light Scattering (DLS) and zeta potential. Scanning Electron Microscopy (SEM) was used to investigate the morphology of the zinc-doped hydroxyapatite (Zn:HAp) nanogel composite and Zn:HAp coatings. The elements Ca, P, O and Zn were found in the Zn:HAp composite. According to the EDX results, the degree of Zn substitution in the structure of Zn:HAp composite was 1.67 wt%. Moreover, the antifungal activity of Zn:HAp_Si and Zn:HAp_Ti against Candida albicans (C. albicans) was evaluated. A decrease in the number of surviving cells was not observed under dark conditions, whereas under daylight and UV light illumination a major decrease in the number of surviving cells was observed.

74. Textural, Structural and Biological Evaluation of Hydroxyapatite Doped with Zinc at Low Concentrations

Authors: Predoi, D; Iconaru, SL; Deniaud, A; Chevallet, M; Michaud-Soret, I; Buton, N; Prodan, AM

Published: MAR 2017, MATERIALS, 10, DOI: 10.3390/ma10030229

The present work was focused on the synthesis and characterization of hydroxyapatite doped with low concentrations of zinc (Zn: HAp) (0.01 < x(Zn) < 0.05). The incorporation of low concentrations of Zn2+ ions in the hydroxyapatite (HAp) structure was achieved by co-precipitation method. The physico-chemical properties of the samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), zeta-potential, and DLS and N2-BET measurements. The results obtained by XRD and FTIR studies demonstrated that doping hydroxyapatite with low concentrations of zinc leads to the formation of a hexagonal structure with lattice parameters characteristic to hydroxyapatite. The XRD studies have also shown that the crystallite size and lattice parameters of the unit cell depend on the substitutions of Ca2+ with Zn2+ in the apatitic structure. Moreover, the FTIR analysis revealed that the water content increases with the increase of zinc concentration. Furthermore, the Energy Dispersive X-ray Analysis (EDAX) and XPS analyses showed that the elements Ca, P, O, and Zn were found in all the Zn: HAp samples suggesting that the synthesized materials were zinc doped hydroxyapatite, Ca10-Zn-x(x)(PO4) (6)(OH), with 0.01 <= x(Zn) <= 0.05. Antimicrobial assays on Staphylococcus aureus and Escherichia coli bacterial strains and HepG2 cell viability assay were carried out.

75. Structural and Antimicrobial Evaluation of Silver Doped Hydroxyapatite- Polydimethylsiloxane Thin Layers

Authors: Iconaru, SL; Chifiriuc, MC; Groza, A

Published: 2017, JOURNAL OF NANOMATERIALS, 2017, DOI: 10.1155/2017/7492515

An Ag:HAp (x(Ag) = 0.5) powder was deposited by thermal evaporation technique as coating on a silicon substrate previously covered with a polydimethylsiloxane (PDMS) layer. The Ag: HAp-PDMS layers were characterized by Scanning ElectronMicroscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), and Fourier Transform Infrared Spectroscopy (FT-IR). By infrared spectroscopy analysis, the phase composition of the Ag: HAp-PDMS layers was investigated. The antimicrobial activity of Ag: HAp-PDMS layers was tested against Escherichia coli, Staphylococcus aureus, and Candida albicans microbial strains. The microbial activity decreases significantly for the surveyed time intervals on Ag: HAp-PDMS layers.

76. Ultrasonic Measurements on Cyclodextrin/Hydroxyapatite Composites for Potential Water Depollution

Authors: Predoi, D; Predoi, MV; Iconaru, SL; El Kettani, MEC; Leduc, D; Prodan, AM

Published: JUN 2017, MATERIALS, 10, DOI: 10.3390/ma10060681

This paper presents structural, morphological and preliminary ultrasonic characterizations of the -Cyclodextrin/hydroxyapatite (CD-HAp) composites synthesized by an adapted co-precipitation method. The structural and morphological properties were evaluated by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDX). The specific surface area, pore size and pore volume were determined using the methods of Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH), respectively. The novelty of our study consists in preliminary ultrasonic measurements conducted on CD-HAp composite, uniformly dispersed in distilled water. The benefit of this non-destructive method was to facilitate and simplify the characterization techniques of nanoparticles. Our experiments proved that the efficiency of lead ion removal by CD-HAp composites depended on the initial concentration of lead. The maximum adsorption capacity of the solid phase, for Pb2+ indicated a higher rate of removal by the CD-HAp_2. These adsorption results bring valuable insight into the beneficial contribution of our compounds, for the removal of heavy metal ions from aqueous solutions. Furthermore, in the present study, was evaluated the toxic effect of lead ions adsorbed by hydroxyapatite from contaminated water on HeLa cells.

77. Physicochemical and antimicrobial properties of silver-doped hydroxyapatite collagen biocomposite

Authors: Predoi, D; Iconaru, SL; Albu, M; Petre, CC; Jiga, G

Published: JUN 2017, POLYMER ENGINEERING AND SCIENCE, 57, 545, DOI: 10.1002/pen.24553

Silver-doped hydroxyapatite (AgHAp) was prepared by co-precipitation method at room temperature. The obtained AgHAp was added in different amounts of collagen gel (AgHApC1 and AgHApC2). Afterward, the gel was lyophilized and the final AgHApC1 and AgHApC2 composite was achieved. The purity, crystallinity, and the phase composition of the AgHAp, AgHApC1, and AgHApC2 samples were evaluated by X-ray diffraction (XRD). The planes corresponding to the 2 values for hydroxyapatite were found in the three samples analyzed in agreement with the crystalline hydroxyapatite. In the Fourier transform infrared (FT-IR) spectra of AgHApC1 and AgHApC2 samples the peak characteristic to the presence of (2) phosphate mode at 472/cm was found. The peaks resulting from the (4) vibration of the P-O mode, (1) symmetric P-O stretching vibration and (3) P-O stretching vibration of PO43- were also evidenced in all the samples. The formation of agglomerated particles with uniform particle size was evidenced by scanning electron microscope (SEM). The uniform distribution of the constituent elements was evidenced by mapping analysis. Furthermore, the strong antibacterial activity of AgHAp, AgHApC1, and AgHApC2 samples against Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus aureus) bacterial strains was shown. The inhibition zone increased drastically with the increase of silver concentration. POLYM. ENG. SCI., 57:537-545, 2017. (c) 2017 Society of Plastics Engineers

78. PROPERTIES OF SAMARIUM DOPED HYDROXYAPATITE THIN FILMS DEPOSITED BY EVAPORATION

Authors: Iconaru, SL; Stanciu, GA; Hristu, R; Ghita, RV

Published: 2017, ROMANIAN REPORTS IN PHYSICS, 69, DOI:

The aim of this study was to investigate the antifungal activity of samarium doped hydroxyapatite (Ca10-xSmx(PO4)(6)(OH)(2), x(Sm) = 0.02 and x(Sm) = 0.05) layers deposited on titanium substrate by a thermal evaporation technique. The morphology of the samarium doped hydroxyapatite layers deposited on a Ti (Ti-Sm:HAp_2 and Ti-Sm: HAp_5) substrate were investigated using scanning electron microscopy (SEM). The antifungal activity of the Sm:HAp layers was assessed using Candida albicans ATCC 10231 fungal strain. The biofilm development of the C. albicans on the Sm: HAp layers was investigated by confocal laser scanning microscopy (CLSM). The results have evidenced a significant inhibition of the fungal cells adherence and biofilm development on the Sm: HAp layers.

79. Enamel Based Composite Layers Deposited on Titanium Substrate with Antifungal Activity

Authors: Iconaru, SL; Prodan, AM; Turculet, CS; Beuran, M; Ghita, RV; Costescu, A; Groza, A; Chifiriuc, MC; Chapon, P; Gaiaschi, S; Hristu, R; Stanciu, GA; Trusca, R; Ganciu, M; Raita, SM; Vineticu, N; Ciobanu, CS

Published: 2016, JOURNAL OF SPECTROSCOPY, 2016, DOI: 10.1155/2016/4361051

The goal of this paper was to investigate the antifungal activity of Enamel layers deposited on titanium substrate (Ti-Enamel) and Enamel layers deposited on titanium substrate previously coated with a vinyl polydimethylsiloxane layer (Ti-PDMS-Enamel). The physicochemical properties were also investigated. The Candida albicans biofilm development on the obtained layers was examined after 24 h, 48 h, and 72 h by confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM) after ethidium bromide staining. A significant inhibition of the fungal adherence and biofilm development was observed on Ti-Enamel layers. The antifungal results demonstrated that the use of new Ti-Enamel composite layers could represent a promising perspective for the prevention of fungal biofilms associated implant infections.

80. BIOLOGICAL STUDIES ON DEXTRIN COATED IRON OXIDE NANOPARTICLES

Authors: Iconaru, SL; Turculet, C; Le Coustumer, P; Bleotu, C; Chifiriuc, MC; Lazar, V; Surugiu, A; Badea, M; Iordache, FM; Soare, M; Prodan, AM

Published: 2016, ROMANIAN REPORTS IN PHYSICS, 68, 1544, DOI:

In this study, dextrin coated iron oxide nanoparticles were obtained using an adapted chemical co-precipitation method. The size and morphology of the dextrin coated iron oxide nanoparticles (DIO-NPs) were analyzed by transmission electron microscopy (TEM). The scanning electron microscopy (SEM) analysis depicted information on the morphology of DIO-NPs. The elemental analysis was conducted by Energy-dispersive X-ray spectroscopy (EDAX). The iron oxide particles coated with dextrin have a spherical shape at nanometric scale with a narrow size distribution. The cytotoxicity assay was performed by quantification of HeLa cells viability, while the antimicrobial activities of the DIO-NPs were determined against ATCC reference and clinical microbial strains, i.e. Gram-positive bacteria (Staphylococcus aureus ATCC 6538) and yeast (Candida albicans 393). The obtained nanoparticles did not have cytotoxic effect on HeLa cells after a 24 h exposure to DIO-NPs and the morphology of the cells was not affected. A low toxic effect on HeLa cells was noticed after 48 h. The minimal inhibitory concentration of DIO-NPs was 1 mg/mL for both tested microbial strains.

81. Magnetite (Fe3O4) nanoparticles as adsorbents for As and Cu removal

Authors: Iconaru, SL; Guegan, R; Popa, CL; Motelica-Heino, M; Ciobanu, CS; Predoi, D

Published: DEC 2016, APPLIED CLAY SCIENCE, 134, 135, DOI: 10.1016/j.clay.2016.08.019

The aim of this study consisted to develop novel synthetic magnetite nanoparticles (nFe(3)O(4)) with preferential reactivity to trace elements (TE) for possible environmental applications as adsorbents. The synthetic magnetite materials obtained through the co-precipitation of both Fe3+ and Fe2+ ions (Fe2+ / Fe3+ = 0.5) were characterized by a set of complementary techniques: X-ray diffraction, transmission and scanning electron microscopy, Fourier transform infrared and Raman spectroscopy, and BET adsorption method. The resulting nFe(3)O(4) displayed a wide specific surface area (100 m(2) g(-1)) with particles reaching a size of about 10 nm, smaller than those of the well-crystallized commercial ones (cFe(3)O(4)) estimated at 80 nm while showing a BET surface area of 6.8 m(2) The adsorption properties of the synthetic nFe(3)O(4) magnetite nanoparticles were characterized and compared to the commercial analogous with the adsorption of both As and Cu. The equilibrium adsorption isotherms were properly fitted with Langmuir and Freundlich equation models and suggested that the developed iron oxides nanoparticles display a certain potential for removal and/or immobilization of TE from contaminated waters and/or soils, with an increase of 69.5% of the adsorbed amount compared to that of the commercial ones. (C) 2016 Elsevier B.V. All rights reserved.

82. Structural Properties and Antifungal Activity against Candida albicans Biofilm of Different Composite Layers Based on Ag/Zn Doped Hydroxyapatite-Polydimethylsiloxanes

Authors: Groza, A; Ciobanu, CS; Popa, CL; Iconaru, SL; Chapon, P; Luculescu, C; Ganciu, M; Predoi, D

Published: APR 2016, POLYMERS, 8, DOI: 10.3390/polym8040131

Modern medicine is still struggling to find new and more effective methods for fighting off viruses, bacteria and fungi. Among the most dangerous and at times life-threatening fungi is Candida albicans. Our work is focused on surface and structural characterization of hydroxyapatite, silver doped hydroxyapatite and zinc doped hydroxyapatite deposited on a titanium substrate previously coated with polydimethylsiloxane (HAp-PDMS, Ag:HAp-PDMS, Zn:HAp-PDMS) by different techniques:Scanning Electron Microscopy (SEM), Glow Discharge Optical Emission Spectroscopy (GDOES) and Fourier Transform Infrared Spectroscopy (FTIR). The morphological studies revealed that the use of the PDMS polymer as an interlayer improves the quality of the coatings. The structural characterizations of the thin films revealed the basic constituents of both apatitic and PDMS structure. In addition, the GD depth profiles indicated the formation of a composite material as well as the successful embedding of the HAp, Zn:HAp and Ag:HAp into the polymer. On the other hand, in vitro evaluation of the antifungal properties of Ag:HAp-PDMS and Zn:HAp-PDMS demonstrated the fungicidal effects of Ag:HAp-PDMS and the potential antifungal effect of Zn:HAp-PDMS composite layers against C. albicans biofilm. The results acquired in this research complete previous research on the potential use of new complex materials produced by nanotechnology in biomedicine.

83. Evaluation of the Antimicrobial Activity of Different Antibiotics Enhanced with Silver-Doped Hydroxyapatite Thin Films

Authors: Predoi, D; Popa, CL; Chapon, P; Groza, A; Iconaru, SL

Published: SEP 2016, MATERIALS, 9, DOI: 10.3390/ma9090778

The inhibitory and antimicrobial effects of silver particles have been known since ancient times. In the last few years, a major health problem has arisen due to pathogenic bacteria resistance to antimicrobial agents. The antibacterial activities of new materials including hydroxyapatite (HAp), silver-doped hydroxyapatite (Ag:HAp) and various types of antibiotics such as tetracycline (T-HAp and T-Ag:HAp) or ciprofloxacin (C-HAp and C-Ag:HAp) have not been studied so far. In this study we reported, for the first time, the preparation and characterization of various thin films based on hydroxyapatite and silver-doped hydroxyapatite combined with tetracycline or ciprofloxacin. The structural and chemical characterization of hydroxyapatite and silver-doped hydroxyapatite thin films has been evaluated by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The morphological studies of the HAp, Ag: HAp, T-HAp, T-Ag: HAp, C-HAp and C-Ag: HAp thin solid films were performed using scanning electron microscopy (SEM). In order to study the chemical composition of the coatings, energy dispersive X-ray analysis (EDX) and glow discharge optical emission spectroscopy (GDOES) measurements have been used, obtaining information on the distribution of the elements throughout the film. These studies have confirmed the purity of the prepared hydroxyapatite and silver-doped hydroxyapatite thin films obtained from composite targets containing Ca10-xAgx(PO4)(6)(OH)(2) with x(Ag) = 0 (HAp) and x(Ag) = 0.2 (Ag: HAp). On the other hand, the major aim of this study was the evaluation of the antibacterial activities of ciprofloxacin and tetracycline in the presence of HAp and Ag: HAp thin layers against Staphylococcus aureus and Escherichia coli strains. The antibacterial activities of ciprofloxacin and tetracycline against Staphylococcus aureus and Escherichia coli test strains increased in the presence of HAp and Ag: HAp thin layers.

84. Sulfur treatment on n-GaSb (100) and surface antibacterial evaluation

Authors: Ghita, R; Iconaru, SL; Frumosu, F; Logofatu, C; Badea, ML; Holban, AM

Published: OCT 16 2015, TOXICOLOGY LETTERS, 238, S199, DOI: 10.1016/j.toxlet.2015.08.599

85. Influence of Thermal Treatment on the Antimicrobial Activity of Silver-Doped Biological Apatite

Authors: Popa, CL; Ciobanu, CS; Voicu, G; Vasile, E; Chifiriuc, MC; Iconaru, SL; Predoi, D

Published: DEC 29 2015, NANOSCALE RESEARCH LETTERS, 10, DOI: 10.1186/s11671-015-1211-x

In this paper, we report the structural and morphological properties of silver-doped hydroxyapatite (AgHAp) with a silver concentration x(Ag) = 0.5 before and after being thermal treated at 600 and 1000 degrees C. The results obtained by X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Raman spectroscopy suggest that the structure of the samples changes gradually, from hydroxyapatite (AgHAp_40) to a predominant beta-TCP structure (AgHAp_1000), achieved when the thermal treatment temperature is 1000 degrees C. In the AgHAp_600 sample, the presence of two phases, HAp and beta-TCP, was highlighted. Also, scanning electron microscopy studies suggest that the shape and dimension of the nanoparticles begin to change when the temperature increases. The antimicrobial activity of the obtained compounds was evaluated against Klebsiella pneumoniae, Staphylococcus aureus, and Candida albicans strains.

86. Antimicrobial Activity Evaluation on Silver Doped Hydroxyapatite/Polydimethylsiloxane Composite Layer

Authors: Ciobanu, CS; Groza, A; Iconaru, SL; Popa, CL; Chapon, P; Chifiriuc, MC; Hristu, R; Stanciu, GA; Negrila, CC; Ghita, RV; Ganciu, M; Predoi, D

Published: 2015, BIOMED RESEARCH INTERNATIONAL, 2015, DOI: 10.1155/2015/926513

The goal of this study was the preparation, physicochemical characterization, and microbiological evaluation of novel hydroxyapatite doped with silver/polydimethylsiloxane (Ag:HAp-PDMS) composite layers. In the first stage, the deposition of polydimethylsiloxane (PDMS) polymer layer on commercially pure Si disks has been produced in atmospheric pressure corona discharges. Finally, the new silver doped hydroxyapatite/polydimethylsiloxane composite layer has been obtained by the thermal evaporation technique. The Ag: HAp-PDMS composite layers were characterized by various techniques, such as Scanning Electron Microscopy (SEM), Glow Discharge Optical Emission Spectroscopy (GDOES), and X-ray photoelectron spectroscopy (XPS). The antimicrobial activity of the Ag:HAp-PDMS composite layer was assessed against Candida albicans ATCC 10231 (ATCC-American Type Culture Collection) by culture based and confirmed by SEM and Confocal Laser Scanning Microscopy (CLSM) methods. This is the first study reporting the antimicrobial effect of the Ag: HAp-PDMS composite layer, which proved to be active against Candida albicans biofilm embedded cells.

87. Evaluation of Samarium Doped Hydroxyapatite, Ceramics for Medical Application: Antimicrobial Activity

Authors: Ciobanu, CS; Iconaru, SL; Popa, CL; Motelica-Heino, M; Predoi, D

Published: 2015, JOURNAL OF NANOMATERIALS, 2015, DOI: 10.1155/2015/849216

Samarium doped hydroxyapatite (Sm:HAp), Ca10-xSmx(PO4)(6)(OH)(2) (HAp), bionanoparticles with different x(Sm) have been successfully synthesized by coprecipitation method. Detailed characterization of samarium doped hydroxyapatite nanoparticles (Sm: HAp-NPs) was carried out using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FTIR). The biocompatibility of samarium doped hydroxyapatite was assessed by cell viability. The antibacterial activity of the Sm: HAp-NPs was tested against Gram-negative bacteria (Pseudomonas aeruginosa and Escherichia coli) andGram-positive bacteria (Enterococcus faecalis and Staphylococcus aureus). A linear increase of antimicrobial activity of P. aeruginosa has been observed when concentrations of Sm: HAp-NPs in the samples with x(Sm) = 0.02 were higher than 0.125 mg/mL. For Sm: HAp-NPs with x(Sm) = 0.05 a significant increase of antibacterial activity on E. coli was observed in the range 0.5-1 mg/mL. For low concentrations of Sm: HAp-NPs (x(Sm) = 0.05) from 0.031 to 0.125 mg/mL a high antibacterial activity on Enterococcus faecalis has been noticed. A growth of the inhibitory effect on S. aureus was observed for all concentrations of Sm: HAp-NPs with x(Sm) = 0.02.

88. Optical properties and antimicrobial activity evaluation of europium/silver doped hydroxyapatite nanoparticles

Authors: Ciobanu, CS; Prodan, AM; Turculet, C; Iordache, F; Iconaru, SL; Popa, CL; Badea, ML; Predoi, D

Published: OCT 16 2015, TOXICOLOGY LETTERS, 238, S198, DOI: 10.1016/j.toxlet.2015.08.595

89. Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

Authors: Iconaru, SL; Chapon, P; Le Coustumer, P; Predoi, D

Published: 2014, SCIENTIFIC WORLD JOURNAL, DOI: 10.1155/2014/165351

In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FTIR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x(Ag) = 0.5 are effective against E. coli and S. aureus after 24 h.

90. Systematic investigation and in vitro biocompatibility studies on mesoporous europium doped hydroxyapatite

Authors: Popa, CL; Ciobanu, CS; Iconaru, SL; Stan, M; Dinischiotu, A; Negrila, CC; Motelica-Heino, M; Guegan, R; Predoi, D

Published: OCT 2014, CENTRAL EUROPEAN JOURNAL OF CHEMISTRY, 12, 1046, DOI: 10.2478/s11532-014-0554-y

This paper reports the systematic investigation of europium doped hydroxyapatite (Eu:HAp). A set of complementary techniques, namely Fourier Transform Infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and the Brunauer-Emmett-Teller (BET) technique were used towards attaining a detailed understanding of Eu:HAp. The XPS analysis confirmed the substitution of Ca ions by Eu ions in the Eu:HAp samples. Secondly, Eu:HAp and pure HAp present type IV isotherms with a hysteresis loop at a relative pressure (P/P-0) between 0.4 and 1.0, indicating the presence of mesopores. Finally, the in vitro biological effects of Eu:HAp nanoparticles were evaluated by focusing on the F-actin filament pattern and heat shock proteins (Hsp) expression in HEK293 human kidney cell line. Fluorescence microscopy studies of the actin protein revealed no changes of the immunolabelling profile in the renal cells cultured in the presence of Eu:HAp nanoparticles. Hsp60, Hsp70 and Hsp90 expressions measured by Western blot analysis were not affected after 24 and 48 hours exposure. Taken together, these results confirmed the lack of toxicity and the biocompatibility of the Eu:HAp nanoparticles. Consequently, the possibility of using these nanoparticles for medical purposes without affecting the renal function can be envisaged.

91. Hydroxyapatite With Environmental Applications

Authors: Popa, CL; Ciobanu, CS; Petre, CC; Motelica-Heino, M; Iconaru, SL; Jiga, G; Predoi, D

Published: 2014, TIMES OF POLYMERS (TOP) AND COMPOSITES 2014, 1599, 321, DOI: 10.1063/1.4876842

The aim of this study was to synthetize new nanoparticles based on methyltrimethoxysilane coated hydroxyapatite (MTHAp) for lead removal in aqueous solutions. The morphological and compositional analysis of MTHAp was investigated by scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled concentration of Pb2+ and at fixed pH of 5. After the removal experiment of Pb2+ ions from solutions, porous hydroxyapatite nanoparticles were transformed into PbMTHAp_5 via the adsorption of Pb2+ ions followed by a cation exchange reaction. Our results demonstrate that the porous hydroxyapatite nanoparticles can be used as an adsorbent for removing Pb2+ ions from aqueous solution.

92. In vivo toxicity studies of superparamagnetic iron oxide nanoparticles in a silica matrix

Authors: Iconaru, SL; Prodan, AM; Ciobanu, CS; Motelica-Heino, M; Predoi, D

Published: SEP 2014, FEBS JOURNAL, 281, 748, DOI:

93. Antimicrobial studies on porous hydroxyapatite used in the environment and biological applications

Authors: Ciobanu, CS; Iconaru, SL; Predoi, D

Published: SEP 2014, FEBS JOURNAL, 281, 730, DOI:

94. Porous Methyltrimethoxysilane Coated Nanoscale-Hydroxyapatite for Removing Lead Ions from Aqueous Solutions

Authors: Ciobanu, CS; Iconaru, SL; Popa, CL; Costescu, A; Motelica-Heino, M; Predoi, D

Published: 2014, JOURNAL OF NANOMATERIALS, 2014, DOI: 10.1155/2014/361061

The aim of this study was to synthetize new porous nanoparticles based on methyltrimethoxysilane coated hydroxyapatite (MTHAp) for lead removal form aqueous solutions. The morphological and compositional analysis of MTHAp were investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled concentration of Pb2+ at a fixed pH value of 3 and 5 respectively. After the removal experiment of Pb2+ ions from solutions, porous hydroxyapatite nanoparticles were transformed into PbMTHAp_3 and PbMTHAp_5 via the adsorption of Pb2+ ions followed by a cation exchange reaction. The X-ray diffraction spectra of PbMTHAp_3 and PbMTHAp_5 revealed that the powders, after removal of the Pb2+ ions, were a mixture of Ca2.5Pb7.5(PO4)(6) (OH) 2, Pb2Ca4(PO4)(2)(SiO4), and Ca-10(PO4)(6)(OH)(2). Our results demonstrate that the porous hydroxyapatite nanoparticles can be used as an adsorbent for removing Pb2+ ions from aqueous solutions.

95. In vivo toxicity studies of dextran coated iron oxide nanoparticles

Authors: Prodan, AM; Iconaru, SL; Popa, CL; Predoi, D

Published: SEP 2014, FEBS JOURNAL, 281, 573, DOI:

96. Toxicity Evaluation following Intratracheal Instillation of Iron Oxide in a Silica Matrix in Rats

Authors: Prodan, AM; Ciobanu, CS; Popa, CL; Iconaru, SL; Predoi, D

Published: 2014, BIOMED RESEARCH INTERNATIONAL, 2014, DOI: 10.1155/2014/134260

Iron oxide-silica nanoparticles (IOSi-NPs) were prepared from a mixture of ferrous chloride tetrahydrate and ferric chloride hexahydrate dropped into a silica xerogel composite. The structure and morphology of the synthesized maghemite nanoparticles into the silica xerogel were analysed by X-ray diffraction measurements, scanning electron microscopy equipped with an energy dispersive X-ray spectrometer, and transmission electron microscopy. The results of the EDAX analysis indicated that the embedded particles were iron oxide nanoparticles. The particle size of IOSi-NPs calculated from the XRD analysis was estimated at around 12.5 nm. The average size deduced from the particle size distribution is 13.7 +/- 0.6 nm, which is in good agreement with XRDanalysis. The biocompatibility of IOSi-NPs was assessed by cell viability and cytoskeleton analysis. Histopathology analysis was performed after 24 hours and 7 days, respectively, from the intratracheal instillation of a solution containing 0.5, 2.5, or 5mg/ kg IOSi-NPs. The pathological micrographs of lungs derived from rats collected after the intratracheal instillation with a solution containing 0.5mg/kg and 2.5mg/ kg IOSi-NPs show that the lung has preserved the architecture of the control specimen with no significant differences. However, even at concentrations of 5mg/ kg, the effect of IOSi-NPS on the lungs was markedly reduced at 7 days post treatment.

97. Antimicrobial activity of samarium doped hydroxyapaptite prepared by co-precipitation method

Authors: Ciobanu, CS; Popa, CL; Iconaru, SL; Predoi, D

Published: SEP 2014, FEBS JOURNAL, 281, 651, DOI:

98. Tetraethyl Orthosilicate Coated Hydroxyapatite Powders for Lead Ions Removal from Aqueous Solutions

Authors: Ghita, RV; Iconaru, SL; Popa, CL; Costescu, A; Le Coustumer, P; Motelica-Heino, M; Ciobanu, CS

Published: 2014, JOURNAL OF NANOMATERIALS, 2014, DOI: 10.1155/2014/176426

The goal of this study was to synthetize and characterize a porous material based on tetraethyl orthosilicate (TEOS) coated hydroxyapatite (HApTh) after removal experiments of Pb2+ ions from aqueous solutions. In order to study the morphology and composition, the samples obtained after removal experiments of Pb2+ ions from aqueous solution with the initial Pb2+ ion concentrations of the aqueous solutions were 0.1g.L-1 (HApTh-50) and 0.9g.L-1 (HApTh-450) have been investigated by scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS), Fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled concentration of Pb2+. After the removal experiment of Pb2+ ions from solutions, porous hydroxyapatite nanoparticles were transformed into HApTh-50 and HApTh-450 due to the adsorption of Pb2+ ions followed by a cation exchange reaction. The obtained results show that the porous HApTh nanopowders could be used for Pb2+ ions removal from aqueous solutions.

99. Magnetic Properties and Biological Activity Evaluation of Iron Oxide Nanoparticles

Authors: Prodan, AM; Iconaru, SL; Chifiriuc, CM; Bleotu, C; Ciobanu, CS; Motelica-Heino, M; Sizaret, S; Predoi, D

Published: 2013, JOURNAL OF NANOMATERIALS, 2013, DOI: 10.1155/2013/893970

The aim of this study was to provide information about the biological properties of iron oxide nanoparticles (IO-NPs) obtained in an aqueous suspension. The IO-NPs were characterized by transmission electron microscopy (TEM). Analysis of hysteresis loops data at room temperature for magnetic IO-NPs sample indicated that the IO-NPs were superparamagnetic at room temperature. The calculated saturation magnetization for magnetic iron oxide was M-s = 18.1 emu/g. The antimicrobial activity of the obtained PMC-NPs was tested against Gram-negative (Pseudomonas aeruginosa 1397, Escherichia coli ATCC 25922), Gram-positive (Enterococcus faecalis ATCC 29212, Bacillus subtilis IC 12488) bacterial as well as fungal (Candida krusei 963) strains. The obtained results suggested that the antimicrobial activity of IO-NPs is dependent on the metallic ions concentrations and on the microbial growth state, either planktonic or adherent. The obtained IO-NPs exhibited no cytotoxic effect on HeLa cells at the active antimicrobial concentrations.

100. Synthesis and Antimicrobial Activity of Silver-Doped Hydroxyapatite Nanoparticles

Authors: Ciobanu, CS; Iconaru, SL; Chifiriuc, MC; Costescu, A; Le Coustumer, P; Predoi, D

Published: 2013, BIOMED RESEARCH INTERNATIONAL, 2013, DOI: 10.1155/2013/916218

The synthesis of nanosized particles of Ag-doped hydroxyapatite with antibacterial properties is of great interest for the development of new biomedical applications.. e aim of this study was the evaluation of Ca10-xAgx(PO4)(6)(OH)(2) nanoparticles (Ag:HAp-NPs) for their antibacterial and antifungal activity. Resistance to antimicrobial agents by pathogenic bacteria has emerged in the recent years and became a major health problem. Here, we report a method for synthesizing Ag doped nanocrystalline hydroxyapatite. A silver-doped nanocrystalline hydroxyapatite was synthesized at 100 degrees C in deionised water. Also, in this paper Ag:HAp-NPs are evaluated for their antimicrobial activity against ram-positive and ram-negative bacteria and fungal strains. The specific antimicrobial activity revealed by the qualitative assay is demonstrating that our compounds are interacting differently with the microbial targets, probably due to the differences in the microbial wall structures.

101. Study on Europium-Doped Hydroxyapatite Nanoparticles by Fourier Transform Infrared Spectroscopy and Their Antimicrobial Properties

Authors: Iconaru, SL; Motelica-Heino, M; Predoi, D

Published: 2013, JOURNAL OF SPECTROSCOPY, 2013, DOI: 10.1155/2013/284285

Fourier transform infrared spectroscopy (FT-IR) analysis was conducted on europium-doped hydroxyapatite, Ca10-xEux (PO4)(6)(OH)(2) nanocrystalline powders (Eu:HAp) with 0 < x(Eu) < 0.2. Antimicrobial studies were also performed for the first time on Eu: HAp. The antimicrobial properties of Eu: HAp nanoparticles with 0 < x(Eu) <= 0.2 on Gram-negative (E. coli ATCC 25922, Pseudomonas aeruginosa 1397) andGram-positive (Staphylococcus aureus 0364, Enterococcus faecalis ATCC 29212) bacteria systems and a species of fungus (Candida albicans ATCC 10231) were reported. Our study demonstrates that the antimicrobial activity of Eu: HAp nanoparticles is dependent on the europium concentration.

102. Physico-chemical and antibacterial studies on silver doped nano-hydroxyapatite

Authors: Ciobanu, CS; Andronescu, E; Prodan, AM; Pall, L; Costescu, A; Le Coustumer, P; Huneau, F; Marutescu, L; Ene, NI; Trusca, R; Barna, ES; Iconaru, SL

Published: JUL-AUG 2013, JOURNAL OF OPTOELECTRONICS AND ADVANCED MATERIALS, 15, 922, DOI:

In this paper we show that preparation of Ag doped hydroxyapatite by an adapted co-precipitation method at 100 C has several advantages over other techniques. Specifically, it can generate highly crystalline nanopowder Ag:HAp which could be used for implantable medical devices. The XRD of HAp (x(Ag) = 0) and Ag:HAp (x(Ag) = 0.05, and x(Ag) = 0.4) also demonstrates that powders obtained by co-precipitation at 100 C exhibit the apatite characteristics with good crystal structure and no new phase or impurity is found. The SEM results suggested that Ag+ doping had little influence on the morphology and dimension of the samples. It can be seen that all the samples consist of elipsoidal particles. The antibactericidal activity of Ag:HAp-NPs with x(Ag) = 0, x(Ag) = 0.05, and x(Ag) = 0.4 on Bacilus and E.coli ESBL 1576 were presented. The Ag:HAp-NPs with x(Ag) = 0.05, and x(Ag) = 0.4 inhibited the biofilm development both by the gram-positive (Staphylococcus aureus 0364) and the gram-negative (Providencia stuartii 1116) strains. On the other hand, our studies have shown that Ag:HAp with x(Ag) = 0 had no antibacterial activity against gram-positive and gram-negative bacteria.

103. Structural properties of silver doped hydroxyapatite and their biocompatibility

Authors: Ciobanu, CS; Iconaru, SL; Pasuk, I; Vasile, BS; Lupu, AR; Hermenean, A; Dinischiotu, A; Predoi, D

Published: APR 1 2013, MATERIALS SCIENCE & ENGINEERING C-MATERIALS FOR BIOLOGICAL APPLICATIONS, 33, 1402, DOI: 10.1016/j.msec.2012.12.042

The aim of this study was to obtain a novel hydroxyapatite-based material with high biocompatibility. The structural properties of the samples were well characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The X-ray diffraction studies revealed the characteristic peaks of hydroxyapatite in each sample. Other phases or impurities were not observed. The scanning electron microscopy observations suggest that the doping components have no influence on the surface morphology of the samples, which reveals a homogeneous aspect of the synthesized particles for all samples. The presence of calcium (Ca), phosphor (P), oxygen (O) and silver (Ag) in the Ag:HAp is confirmed by energy dispersive X-ray (EDAX) and X-ray Photoelectron Spectroscopy analyses. Nanocrystalline silver doped HAp stimulated viability and potentiated the activation of murine macrophages. (C) 2012 Elsevier B.V. All rights reserved.

104. Fabrication, Characterization, and Antimicrobial Activity, Evaluation of Low Silver Concentrations in Silver-Doped Hydroxyapatite Nanoparticles

Authors: Costescu, A; Ciobanu, CS; Iconaru, SL; Ghita, RV; Chifiriuc, CM; Marutescu, LG; Predoi, D

Published: 2013, JOURNAL OF NANOMATERIALS, 2013, DOI: 10.1155/2013/194854

The aim of this study was the evaluation of (Ca10-x Ag-x)(PO4)(6) (OH)(2) nanoparticles (Ag:HAp-NPs) for their antibacterial and antifungal activity. Resistance to antimicrobial agents by pathogenic bacteria has emerged in the recent years as a major public health problem worldwide. In this paper, we report a comparison of the antimicrobial activity of low concentrations silver-doped hydroxyapatite nanoparticles. Thesilver-doped nanocrystalline hydroxyapatite powder was synthesized at 100 degrees C indeionised water. The as-prepared Ag: Hap nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR, and FT-Raman spectroscopy. X-ray diffraction (XRD) studies demonstrate that powders obtained by coprecipitation at 100 degrees C exhibit the apatite characteristics with good crystal structure, without any new phase or impurities found. FT-IR and FT-Raman spectroscopy revealed the presence of the various vibrational modes corresponding to phosphates and hydroxyl groups and the absence of any band characteristic to silver. The specific microbiological assays demonstrated that Ag: HAp-NPs exhibited antimicrobial features, but interacted differently with the Gram-positive, Gram-negative bacterial and fungal tested strains.

105. Anti-biofilm activity of maghemite nanoparticles coated with dextran

Authors: Ciobanu, CS; Iconaru, SL; Predoi, D

Published: JUL 2013, FEBS JOURNAL, 280, 359, DOI:

106. Antimicrobial activity of silver doped hydroxyapaptite thin films

Authors: Ciobanu, CS; Iconaru, SL; Chapon, P; Predoi, D

Published: JUL 2013, FEBS JOURNAL, 280, 360, DOI:

107. Synthesis and Antibacterial and Antibiofilm Activity of Iron Oxide Glycerol Nanoparticles Obtained by Coprecipitation Method

Authors: Iconaru, SL; Prodan, AM; Le Coustumer, P; Predoi, D

Published: 2013, JOURNAL OF CHEMISTRY, 2013, DOI: 10.1155/2013/412079

The glycerol iron oxide nanoparticles (GIO-NPs) were obtained by an adapted coprecipitation method. The X-ray diffraction (XRD) studies demonstrate that GIO-NPs were indexed into the spinel cubic lattice with a lattice parameter of 0.835 nm. The refinement of XRD spectra indicated that no other phases except maghemite were detected. The adsorption of glycerol on iron oxide nanoparticles was investigated by Fourier transform infrared (FTIR) spectroscopy. On the other hand, this work implicated the use of GIO-NPs in antibacterial studies. The results indicate that, in the case of P.aeruginosa 1397 biofilms, at concentrations from 0.01 mg/mL to 0.625 mg/mL, the glycerol iron oxide inhibits the ability of this strain to develop biofilms on the inert substratum.

108. Vibrational Investigations of Silver-Dovep Hydroxyapatite with Antibacterial Properties

Authors: Ciobanu, CS; Iconaru, SL; Le Coustumer, P; Predoi, D

Published: 2013, JOURNAL OF SPECTROSCOPY, 2013, DOI: 10.1155/2013/471061

Silver-doped hydroxyapatite (Ag:HAp) was obtained by coprecipitation method. Transmission electron microscopy (TEM), infrared, and Raman analysis confirmed the development of Ag:HAp with good crystal structure. Transmission electron microscopy analysis showed an uniform ellipsoidal morphology with particles from 5 nm to 15 nm. The main vibrational bands characteristic to HAp were identified. The bands assigned to phosphate vibrational group were highlighted in infrared and Raman spectra. The most intense peak Raman spectrum is the narrow band observed at 960 cm(-1). In this article Ag:Hap-NPs were also evaluated for their antimicrobial activities against gram-positive, gram-negative, and fungal strains. The specific antimicrobial activity revealed by the qualitative assay demonstrates that our compounds are interacting differently with the microbial targets.

109. Structural Characterization and Magnetic Properties of Iron Oxides Biological Polymers

Authors: Iconaru, SL; Ciobanu, CS; Le Coustumer, P; Predoi, D

Published: APR 2013, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 26, 855, DOI: 10.1007/s10948-012-1855-z

Iron oxide nanoparticles (IONs) coated with different biological (dextran, sucrose) polymers have been synthesized by the coprecipitation method. Biological polymers coated iron oxide nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM). Zero field cooled and field cooled magnetizations measurements are also reported. We present a preliminary study of the influence of biological polymer on the interaction effects in powders. The temperature, T (max), of the maximum, increased from 25 K (dextran) to 52 K (sucrose). These values are due to the decrease of interparticle interactions, mainly as a result of the interparticle distance increase.

110. Iron Oxide Magnetic Nanoparticles: Characterization and Toxicity Evaluation by In Vitro and In Vivo Assays

Authors: Prodan, AM; Iconaru, SL; Ciobanu, CS; Chifiriuc, MC; Stoicea, M; Predoi, D

Published: 2013, JOURNAL OF NANOMATERIALS, 2013, DOI: 10.1155/2013/587021

The aim of this study was to evaluate the biological properties of iron oxide nanoparticles (IO-NPs) obtained in the aqueous suspension. The iron oxide nanoparticles were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The biocompatibility of the iron oxide was demonstrated by the in vitro quantification of HeLa cells viability using propidium iodide (PI) and fluorescein diacetate (FdA) and the MTT colorimetric assay. The toxicity of small size iron oxide nanoparticles was also evaluated by means of histological examination on male Brown Norway rats after intraperitoneal injection. At the tested concentrations, the nanoparticles proved to be not cytotoxic on HeLa cells. The rat's behavior, as well as the histopathological aspect of liver, kidney, lung, and spleen tissues at 48 h after intraperitoneal injection did not present any modifications. The in vivo and in vitro assays suggested that the IO-NPs could be further used for developing new in vivo medical applications.

111. The antimicrobial activity of fabricated iron oxide nanoparticles

Authors: Iconaru, SL; Ciobanu, CS; Prodan, AM; Predoi, D

Published: SEP 2012, FEBS JOURNAL, 279, 98, DOI:

112. Biomedical properties and preparation of iron oxide-dextran nanostructures by MAPLE technique

Authors: Ciobanu, CS; Iconaru, SL; Gyorgy, E; Radu, M; Costache, M; Dinischiotu, A; Le Coustumer, P; Lafdi, K; Predoi, D

Published: MAR 13 2012, CHEMISTRY CENTRAL JOURNAL, 6, DOI: 10.1186/1752-153X-6-17

Background: In this work the chemical structure of dextran-iron oxide thin films was reported. The films were obtained by MAPLE technique from composite targets containing 10 wt. % dextran with 1 and 5 wt.% iron oxide nanoparticles (IONPs). The IONPs were synthesized by co-precipitation method. A KrF* excimer laser source (lambda = 248 nm, tau(FWHM)congruent to 25 ns, nu = 10 Hz) was used for the growth of the hybrid, iron oxide NPs-dextran thin films. Results: Dextran coated iron oxide nanoparticles thin films were indexed into the spinel cubic lattice with a lattice parameter of 8.36 angstrom. The particle sized calculated was estimated at around 7.7 nm. The XPS shows that the binding energy of the Fe 2p(3/2) of two thin films of dextran coated iron oxide is consistent with Fe3+ oxides. The atomic percentage of the C, O and Fe are 66.71, 32.76 and 0.53 for the films deposited from composite targets containing 1 wt.% maghemite and 64.36, 33.92 and 1.72 respectively for the films deposited from composite targets containing 5 wt.% maghemite. In the case of cells cultivated on dextran coated 5% maghemite gamma-Fe2O3, the number of cells and the level of F-actin were lower compared to the other two types of thin films and control. Conclusions: The dextran-iron oxide continuous thin films obtained by MAPLE technique from composite targets containing 10 wt.% dextran as well as 1 and 5 wt.% iron oxide nanoparticles synthesized by co-precipitation method presented granular surface morphology. Our data proved a good viability of Hep G2 cells grown on dextran coated maghemite thin films. Also, no changes in cells morphology were noticed under phase contrast microscopy. The data strongly suggest the potential use of iron oxide-dextran nanocomposites as a potential marker for biomedical applications.

113. Antibacterial activity of silver-doped hydroxyapatite nanoparticles against gram-positive and gram-negative bacteria

Authors: Ciobanu, CS; Iconaru, SL; Le Coustumer, P; Constantin, LV; Predoi, D

Published: JUN 21 2012, NANOSCALE RESEARCH LETTERS, 7, DOI: 10.1186/1556-276X-7-324

Ag-doped nanocrystalline hydroxyapatite nanoparticles (Ag:HAp-NPs) (Ca10-x Ag (x) (PO4)(6)(OH)(2), x (Ag) = 0.05, 0.2, and 0.3) with antibacterial properties are of great interest in the development of new products. Coprecipitation method is a promising route for obtaining nanocrystalline Ag:HAp with antibacterial properties. X-ray diffraction identified HAp as an unique crystalline phase in each sample. The calculated lattice constants of a = b = 9.435 , c = 6.876 for x (Ag) = 0.05, a = b = 9.443 , c = 6.875 for x (Ag) = 0.2, and a = b = 9.445 , c = 6.877 for x (Ag) = 0.3 are in good agreement with the standard of a = b = 9.418 , c = 6.884 (space group P6(3)/m). The Fourier transform infrared and Raman spectra of the sintered HAp show the absorption bands characteristic to hydroxyapatite. The Ag:HAp nanoparticles are evaluated for their antibacterial activity against Staphylococcus aureus, Klebsiella pneumoniae, Providencia stuartii, Citrobacter freundii and Serratia marcescens. The results showed that the antibacterial activity of these materials, regardless of the sample types, was greatest against S. aureus, K. pneumoniae, P. stuartii, and C. freundii. The results of qualitative antibacterial tests revealed that the tested Ag:HAp-NPs had an important inhibitory activity on P. stuartii and C. freundii. The absorbance values measured at 490 nm of the P. stuartii and C. freundii in the presence of Ag:HAp-NPs decreased compared with those of organic solvent used (DMSO) for all the samples (x (Ag) = 0.05, 0.2, and 0.3). Antibacterial activity increased with the increase of x (Ag) in the samples. The Ag:HAp-NP concentration had little influence on the bacterial growth (P. stuartii).

114. SYNTHESIS OF PLANT MEDIATED GOLD NANOPARTICLES USING FLOWER EXTRACTS OF CARTHAMUS TINCTORIUS L. (SAFFLOWER) AND EVALUATION OF THEIR BIOLOGICAL ACTIVITIES

Authors: Nagaraj, B; Malakar, B; Divya, TK; Krishnamurthy, NB; Liny, P; Dinesh, R; Iconaru, SL; Ciobanu, CS

Published: JUL-SEP 2012, DIGEST JOURNAL OF NANOMATERIALS AND BIOSTRUCTURES, 7, 1296, DOI:

The ecofriendly synthesis of nanoparticles through various biological sources helps in exploring various herbs. Generally, nanoparticles are prepared by a variety of chemical methods which are not environmentally friendly. In this report we use aqueous extracts of Carthamus Tinctorius L. (Safflower) flowers for the synthesis of gold (Au) nanoparticles. A rapid and convenient method was considered for the synthesis of gold nanoparticles by reduction with auric chloride. UV-visible spectroscopy studies were carried out to assess the formation of Au nanoparticles. Transmission electron microscopy (TEM) was used to characterize the Au nanoparticles. TEM image divulges that nano triangle and spherical shaped gold nanoparticles are formed with polydispersed size, and the sizes are in the range of 40 nm to 200 nm. The antimicrobial activity of gold nanoparticles was performed on various gram negative bacteria and fungus. The gold nanoparticles showed more inhibitory activity on pathogenic gram negative bacteria than fungus.

115. Synthesis and characterization of polysaccharide-maghemite composite nanoparticles and their antibacterial properties

Authors: Iconaru, SL; Prodan, AM; Motelica-Heino, M; Sizaret, S; Predoi, D

Published: OCT 22 2012, NANOSCALE RESEARCH LETTERS, 7, DOI: 10.1186/1556-276X-7-576

The aim of this study was to obtain saccharide (dextran and sucrose)-coated maghemite nanoparticles with antibacterial activity. The polysaccharide-coated maghemite nanoparticles were synthesized by an adapted coprecipitation method. X-ray diffraction (XRD) studies demonstrate that the obtained polysaccharide-coated maghemite nanoparticles can be indexed into the spinel cubic lattice with a lattice parameter of 8.35 angstrom. The refinement of XRD spectra indicated that no other phases except the maghemite are detectable. The characterization of the polysaccharide-coated maghemite nanoparticles by various techniques is described. The antibacterial activity of these polysaccharide-coated maghemite nanoparticles (NPs) was tested against Pseudomonas aeruginosa 1397, Enterococcus faecalis ATCC 29212, Candida krusei 963, and Escherichia coli ATCC 25922 and was found to be dependent on the polysaccharide type. The antibacterial activity of dextran-coated maghemite was significantly higher than that of sucrose-coated maghemite. The antibacterial studies showed the potential of dextran-coated iron oxide NPs to be used in a wide range of medical infections.

116. BIOCOMPATIBLE MAGNETIC IRON OXIDE NANOPARTICLES DOPED DEXTRAN THIN FILMS PRODUCED BY SPIN COATING DEPOSITION SOLUTION

Authors: Iconaru, SL; Andronescu, E; Ciobanu, CS; Prodan, AM; Le Coustumer, P; Predoi, D

Published: JAN-MAR 2012, DIGEST JOURNAL OF NANOMATERIALS AND BIOSTRUCTURES, 7, 409, DOI:

Magnetic iron oxide nanoparticles (MION) doped dextran thin films for biomedical applications have been deposited onto the glass substrate by spin coating method. To understand the influence of the MION doping dextran on physico-chemical properties was conducted. The particle concentration in the samples defined as the oxide/dextran mass ratio, R was 1 and 5. MION -dextran thin films were charcacterized by various techniques such as X-ray Photoelectron Spectroscopy (XPS), Glow Discharge Optical Emission Spectroscopy (GDOES), Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Attachment (EDAX). These techniques have allowed the structural elucidation of polysaccharides thin films. The second derivative FT-IR spectra showed clearly that the polysaccharides bands. The biocompatibility of the maghemite-dextran thin films was demonstrated using MTT test, with the aid of hFOB 1.19 osteoblats cells. To evaluate cell proliferation rate quantitative by the hFOB 1.19 cells on HAp samples were cultured to 4 days. Cellular morphology was investigated using FESEM to obtain qualitative information of osteoblast cells on MION-dextran thin films. The data stronlgy suggest the potential use of iron oxide-dextran nanocomposite as a poetinal marker for or biomedical applications.

117. Synthesis, Structure, and Luminescent Properties of Europium-Doped Hydroxyapatite Nanocrystalline Powders

Authors: Ciobanu, CS; Iconaru, SL; Massuyeau, F; Constantin, LV; Costescu, A; Predoi, D

Published: 2012, JOURNAL OF NANOMATERIALS, 2012, DOI: 10.1155/2012/942801

The luminescent europium-doped hydroxyapatite (Eu:HAp, Ca10-xEux(PO4)(6)(OH)(2)) with 0 <= x <= 0.2 nanocrystalline powders was synthesized by coprecipitation. The structural, morphological, and textural properties were well characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The vibrational studies were performed by Fourier transform infrared, Raman, and photoluminescence spectroscopies. The X-ray diffraction analysis revealed that hydroxyapatite is the unique crystalline constituent of all the samples, indicating that Eu has been successfully inserted into the HAp lattice. Eu doping inhibits IIAp crystallization, leading to a decrease of the average crystallite size from around 20 nm in the undoped sample to around 7 nm in the sample with the highest Eu concentration. Furthermore, the samples show the characteristic D-5(0) -> F-7(0) transition observed at 578 nm related to Eu3+ ions distributed on Ca2+ sites of the apatitic structure.

118. EUROPIUM DOPED HYDROXYAPATITE FOR APPLICATIONS IN ENVIRONMENTAL FIELD

Authors: Constantin, LV; Iconaru, S; Ciobanu, CS

Published: 2012, ROMANIAN REPORTS IN PHYSICS, 64, 794, DOI:

Due to the extensive use of new technologies in agricultural and industrial field the soil and groundwater were severely polluted with elements that may pose a serious threat to the environment. For that purpose studies concerning new materials that can be successfully used for removal of heavy metals and other toxic elements from contaminated soil and water were conducted. The attention of the scientific studies were focused on the family of calcium phosphates, with a particular interest in hydroxyapatite (HAp), with general formula Ca-10(PO4)(6)(OH)(2), due to the exquisite ability of adsorbing heavy element ions in aqueous conditions. This study focuses on synthesizing nanocrystalline hydroxyapatite powders with controllable parameters and very good stoechiometry. The structure, morphology and optical properties were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FT-IR).

119. Assessing toxicity of two types of magnetite nanoparticles in human hepatocarcinoma cells

Authors: Radu, M; Iconaru, SL; Predoi, D; Costache, M; Dinischiotu, A

Published: SEP 2012, FEBS JOURNAL, 279, 205, DOI:

120. Characterization of Sucrose Thin Films for Biomedical Applications

Authors: Iconaru, SL; Ungureanu, F; Costescu, A; Costache, M; Dinischiotu, A; Predoi, D

Published: 2011, JOURNAL OF NANOMATERIALS, 2011, DOI: 10.1155/2011/291512

Sucrose is a natural osmolyte accumulated in the cells of organisms as they adapt to environmental stress. In vitro sucrose increases protein stability and forces partially unfolded structures to refold. Thin films of sucrose (C12H22O11) were deposited on thin cut glass substrates by the thermal evaporation technique (P similar to 10(-5) torr). Characteristics of thin films were put into evidence by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Photoelectron Spectroscopy (XPS), scanning electron microscopy (SEM), and differential thermal analysis and thermal gravimetric analysis (TG/DTA). The experimental results confirm a uniform deposition of an adherent layer. In this paper we present a part of the characteristics of sucrose thin films deposited on glass in medium vacuum conditions, as a part of a culture medium for osteoblast cells. Osteoblast cells were used to determine proliferation, viability, and cytotoxicity interactions with sucrose powder and sucrose thin films. The osteoblast cells have been provided from the American Type Culture Collection (ATCC) Centre. The outcome of this study demonstrated the effectiveness of sucrose thin films as a possible nontoxic agent for biomedical applications.

121. EUROPIUM CONCENTRATION EFFECT OF EUROPIUM DOPED HYDROXYAPATITE ON PROLIFERATION OF OSTEOBLAST CELLS

Authors: Frumosu, F; Iconaru, SL; Predoi, D

Published: OCT-DEC 2011, DIGEST JOURNAL OF NANOMATERIALS AND BIOSTRUCTURES, 6, 1865, DOI:

The aim of this paper is the preparation and characterization of hydroxyapatite doped with europium (Eu3+, Eu:Hap). The nanopowders were obtained by coprecipitation method and analyzed through infrared spectroscopy (FT-IR) and Fourier transform Raman spectroscopy (FT-Raman). The preliminary results reveal the nanometric dimension of the particles and indicate that Eu3+ has been introduced into the framework of HAp. The Eu concentration effects of nano Eu: HAp were studied on human osteoblast MG 63 cells in vitro. Our results demonstrate that cell proliferation is not related to the Eu concentration in the HAp particles. This work provides an interesting view of the role of nano Eu: HAp as ideal biomedical materials in future clinical applications.

122. Physico-chemical Properties of Iron-oxide-dextrin Thin Films

Authors: Ciobanu, CS; Andronescu, E; Pall, L; Iconaru, SL; Gyorgy, E; Predoi, D

Published: DEC 2010, REVISTA DE CHIMIE, 61, 1211, DOI:

Iron oxide nanoparticles were synthesized in the presence of dextrin. The adsorption process of different dextrin molecules onto the surface of in water dispersed iron-oxide nanoparticles has been investigated to optimize the preparation of iron oxide magnetic fluids. An average iron oxide core size of 8 nm was found by transmission electron microscopy (TEM) for the samples. Scanning electron microscopy (SEM) micro-structural studies revealed a spherical shape of the particles. X-ray phase analysis revealed spinel structure of the iron oxide particles. The attachment of the dextrin on the particle surface was investigated by FTIR spectrometry. The dextrin coated iron oxide nanoparticles were used as targets in Pulsed Laser Deposition (PLD) experiments for thin films synthesis.

Dr. Simona ICONARU

Scientific Researcher III

Publications

1. Biocompatibility and Osteogenic Activity of Samarium-Doped Hydroxyapatite-Biomimetic Nanoceramics for Bone Regeneration Applications

2. Sodium bicarbonate-hydroxyapatite used for removal of lead ions from aqueous solution

3. Physico-Chemical and Antimicrobial Features of Magnesium Doped Hydroxyapatite Nanoparticles in Polymer Matrix

4. Exploring the physicochemical traits, antifungal capabilities, and 3D spatial complexity of hydroxyapatite with Ag+-Mg2+substitution in the biocomposite thin films

5. Copper doped hydroxyapatite nanocomposite thin films: synthesis, physico-chemical and biological evaluation

6. New Physico-Chemical Analysis of Magnesium-Doped Hydroxyapatite in Dextran Matrix Nanocomposites

7. Development of Novel Biocomposites with Antimicrobial-Activity-Based Magnesium-Doped Hydroxyapatite with Amoxicillin

8. Novel Antimicrobial Agents Based on Zinc-Doped Hydroxyapatite Loaded with Tetracycline

9. Physico-Chemical and Biological Features of Fluorine-Substituted Hydroxyapatite Suspensions

10. A new porous composite hydroxyapatite/chitosan/microcrystalline-cellulose: synthesis, characterization and application to the adsorption of Eriochrome Black T

11. Synthesis, characterization, and antifungal properties of chrome-doped hydroxyapatite thin films

12. Physico-Chemical Properties of Copper-Doped Hydroxyapatite Coatings Obtained by Vacuum Deposition Technique

13. Morphological and fractal features of cancer cells anchored on composite layers based on magnesium-doped hydroxyapatite loaded in chitosan matrix

14. Hydroxyapatite Nanopowders for Effective Removal of Strontium Ions from Aqueous Solutions

15. Salvia officinalis-Hydroxyapatite Nanocomposites with Antibacterial Properties

16. Influence of the Biological Medium on the Properties of Magnesium Doped Hydroxyapatite Composite Coatings

17. In Vitro and In Vivo Biological Assays of Dextran Coated Iron Oxide Aqueous Magnetic Fluids

18. Complex Evaluation of Nanocomposite-Based Hydroxyapatite for Biomedical Applications

19. Development of Novel Tetracycline and Ciprofloxacin Loaded Silver Doped Hydroxyapatite Suspensions for Biomedical Applications

20. Response of the Endogenous Antioxidant Defense System Induced in RAW 264.7 Macrophages upon Exposure to Dextran-Coated Iron Oxide Nanoparticles

21. Biocomposite Coatings Doped with Magnesium and Zinc Ions in Chitosan Matrix for Antimicrobial Applications

22. Studies of New Layer Formation on the Surface of Zinc Doped Hydroxyapatite/Chitosan Composite Coatings in Biological Medium

23. Studies of the Tarragon Essential Oil Effects on the Characteristics of Doped Hydroxyapatite/Chitosan Biocomposites

24. Novel Dextran Coated Cerium Doped Hydroxyapatite Thin Films

25. Development of Silver Doped Hydroxyapatite Thin Films for Biomedical Applications

26. Impact of Gamma Irradiation on the Properties of Magnesium-Doped Hydroxyapatite in Chitosan Matrix

27. Physicochemical Characterization of Europium-Doped Hydroxyapatite Thin Films with Antifungal Activity

28. The Effects of Electron Beam Irradiation on the Morphological and Physicochemical Properties of Magnesium-Doped Hydroxyapatite/Chitosan Composite Coatings

29. Physicochemical and Biological Evaluation of Chitosan-Coated Magnesium-Doped Hydroxyapatite Composite Layers Obtained by Vacuum Deposition

30. Iron-Oxide-Nanoparticles-Doped Polyaniline Composite Thin Films

31. Fabrication and Physico-Chemical Properties of Antifungal Samarium Doped Hydroxyapatite Thin Films

32. Preparation of Porous Hydroxyapatite Using Cetyl Trimethyl Ammonium Bromide as Surfactant for the Removal of Lead Ions from Aquatic Solutions

33. Investigation of Spin Coating Cerium-Doped Hydroxyapatite Thin Films with Antifungal Properties

34. Fabrication of Novel Chitosan-Hydroxyapatite Nanostructured Thin Films for Biomedical Applications

35. Multi-Level Evaluation of UV Action upon Vitamin D Enhanced, Silver Doped Hydroxyapatite Thin Films Deposited on Titanium Substrate

36. Nitrogen and Bromide Co-Doped Hydroxyapatite Thin Films with Antimicrobial Properties

37. Biocompatibility and Antibiofilm Properties of Samarium Doped Hydroxyapatite Coatings: An In Vitro Study

38. Preparation and Characterization of Dextran Coated Iron Oxide Nanoparticles Thin Layers

39. The Physico-Chemical Properties and Exploratory Real-Time Cell Analysis of Hydroxyapatite Nanopowders Substituted with Ce, Mg, Sr, and Zn (0.5-5 at.%)

40. Development of Iron-Doped Hydroxyapatite Coatings

41. Removal and Oxidation of As(III) from Water Using Iron Oxide Coated CTAB as Adsorbent

42. Multifunctional Hydroxyapatite Coated with Arthemisia absinthium Composites

43. Development of Cerium-Doped Hydroxyapatite Coatings with Antimicrobial Properties for Biomedical Applications

44. Dextran-Thyme Magnesium-Doped Hydroxyapatite Composite Antimicrobial Coatings

45. Obtaining and Characterizing Thin Layers of Magnesium Doped Hydroxyapatite by Dip Coating Procedure

46. Antimicrobial Properties of Samarium Doped Hydroxyapatite Suspensions and Coatings

47. Physico-Chemical Properties and In Vitro Antifungal Evaluation of Samarium Doped Hydroxyapatite Coatings

48. Chitosan-Hydroxyapatite Composite Layers Generated in Radio Frequency Magnetron Sputtering Discharge: From Plasma to Structural and Morphological Analysis of Layers

49. Fabrication of Silver- and Zinc-Doped Hydroxyapatite Coatings for Enhancing Antimicrobial Effect

50. Silver-Doped Hydroxyapatite Thin Layers Obtained by Sol-Gel Spin Coating Procedure

51. Peppermint Essential Oil-Doped Hydroxyapatite Nanoparticles with Antimicrobial Properties

52. The Effect of the Ionizing Radiation on Hydroxyapatite-Polydimethylsiloxane Layers

53. Preparations of Silver/Montmorillonite Biocomposite Multilayers and Their Antifungal Activity

54. Biocompatible Layers Obtained from Functionalized Iron Oxide Nanoparticles in Suspension

55. Photoluminescent Hydroxylapatite: Eu3+ Doping Effect on Biological Behaviour

56. Synthesis, Characterization, and Antimicrobial Activity of Magnesium-Doped Hydroxyapatite Suspensions

57. Zinc Doped Hydroxyapatite Thin Films Prepared by Sol-Gel Spin Coating Procedure

58. Evaluation of Antibacterial Activity of Zinc-Doped Hydroxyapatite Colloids and Dispersion Stability Using Ultrasounds

59. Dextran-Coated Zinc-Doped Hydroxyapatite for Biomedical Applications

60. Commercial Hydroxyapatite Powders for Lead Removal from Aqueous Solution

61. Antimicrobial Studies on Iron Oxide-Dextran Colloidal Suspension

62. Physico-Chemical Characteristics and Antimicrobial Studies of Silver Doped Hydroxyapatite

63. Properties of Basil and Lavender Essential Oils Adsorbed on the Surface of Hydroxyapatite

64. Bioceramic Layers with Antifungal Properties

65. Fabrication and Characterization of Iron Oxide Dextran Composite Layers

66. Removal of Zinc Ions Using Hydroxyapatite and Study of Ultrasound Behavior of Aqueous Media

67. Influence of Ionizing Radiations on Structural and Antibacterial Properties of Hydroxyapatite-Polydimethylsiloxane Layers

68. Application of Biocompatible Magnetite Nanoparticles for the Removal of Arsenic and Copper from Water

69. Adsorption of Pb (II) Ions onto Hydroxyapatite Nanopowders in Aqueous Solutions

70. Antimicrobial Activity of New Materials Based on Lavender and Basil Essential Oils and Hydroxyapatite

71. Development of Zinc-Doped Hydroxyapatite by Sol-Gel Method for Medical Applications

72. ZnHAp Thin Films for Medical Applications

73. Structural Characterization and Antifungal Studies of Zinc-Doped Hydroxyapatite Coatings

74. Textural, Structural and Biological Evaluation of Hydroxyapatite Doped with Zinc at Low Concentrations

75. Structural and Antimicrobial Evaluation of Silver Doped Hydroxyapatite- Polydimethylsiloxane Thin Layers

76. Ultrasonic Measurements on Cyclodextrin/Hydroxyapatite Composites for Potential Water Depollution

77. Physicochemical and antimicrobial properties of silver-doped hydroxyapatite collagen biocomposite