Biological and Physicochemical Analysis of Sr-Doped Hydroxyapatite/Chitosan Composite Layers.

In this work results are presented on the evaluation of HAp, HApSr, HAp_CS, and HApSr_CS layers deposited on Ti substrates regarding L929 cell viability and cytotoxicity as well as antimicrobial activity against Staphylococcus aureus, in connection with their physicochemical properties. The HAp and HApSr layers generated by radio-frequency magnetron sputtering technique were further covered with chitosan by a matrix-assisted pulsed laser evaporation technique. During the plasma depositions, the Ti substrates were heated externally by a home-made oven above 100 °C. The HApSr_CS layers generated on the unpolished Ti substrates at 100 °C and 400 °C showed the highest biocompatibility properties and antimicrobial activity against Staphylococcus aureus. The morphology of the layer surfaces, revealed by scanning electron microscopy, is dependent on substrate temperature and substrate surface roughness. The optically polished surfaces of Ti substrates revealed grain-like and microchannel structure morphologies of the layers deposited at 25 °C substrate temperature and 400 °C, respectively. Chitosan has no major influence on HAp and HApSr layer surface morphologies. X-ray photoelectron spectroscopy indicated the presence of Ca 2p3/2 peak characteristic of the HAp structure even in the case of the HApSr_CS samples generated at a 400 °C substrate temperature. Fourier transform infrared spectroscopy investigations showed shifts in the wavenumber positions of the P-O absorption bands as a function of Sr or chitosan presence in the HAp layers generated at 25, 100, and 400 °C substrate temperatures.

Spectral Analysis of Strontium-Doped Calcium Phosphate/Chitosan Composite Films.

Strontium-doped calcium phosphate/chitosan films were synthetized on silicon substrates using the radio-frequency magnetron sputtering technique and the matrix-assisted pulsed laser evaporation technique. The deposition conditions associated with the radio-frequency magnetron sputtering discharge, in particular, include the high temperature at the substrate, which promotes the formation of strontium-doped tetra calcium phosphate layers. The physical and chemical processes associated with the deposition of chitosan on strontium-doped calcium phosphate layers were investigated using Fourier Transform Infrared Spectroscopy, Energy Dispersive X-ray Spectroscopy, and Scanning Electron Microscopy. Mass spectrometry coupled with laser induced ablation of the composite films proved to be a useful tool in the detection of the molecular ions characteristic to chitosan chemical structure.

Calcium Phosphates-Chitosan Composite Layers Obtained by Combining Radio-Frequency Magnetron Sputtering and Matrix-Assisted Pulsed Laser Evaporation Techniques.

In this work, we report the synthesis of calcium phosphate-chitosan composite layers. Calcium phosphate layers were deposited on titanium substrates by radio-frequency magnetron sputtering technique by varying the substrate temperature from room temperature (25 °C) up to 100 and 300 °C. Further, chitosan was deposited by matrix-assisted pulsed laser evaporation technique on the calcium phosphate layers. The temperature at the substrate during the deposition process of calcium phosphate layers plays an important role in the embedding of chitosan, as scanning electron microscopy analysis showed. The degree of chitosan incorporation into the calcium phosphate layers significantly influence the physico-chemical properties and the adherence strength of the resulted layers to the substrates. For example, the decreases of Ca/P ratio at the addition of chitosan suggests that a calcium deficient hydroxyapatite structure is formed when the CaP layers are generated on Ti substrates kept at room temperature during the deposition process. The Fourier transform infrared spectroscopy analysis of the samples suggest that the PO43-/CO32- substitution is possible. The X-ray diffraction spectra indicated that the crystalline structure of the calcium phosphate layers obtained at the 300 °C substrate temperature is disturbed by the addition of chitosan. The adherence strength of the composite layers to the titanium substrates is diminished after the chitosan deposition. However, no complete exfoliation of the layers was observed.

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

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.

Novel Dextran Coated Cerium Doped Hydroxyapatite Thin Films.

Dextran coated cerium doped hydroxyapatite (Ca10-xCex(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 ν1, ν3, and ν4 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.

Polymeric Coatings and Antimicrobial Peptides as Efficient Systems for Treating Implantable Medical Devices Associated-Infections.

Many infections are associated with the use of implantable medical devices. The excessive utilization of antibiotic treatment has resulted in the development of antimicrobial resistance. Consequently, scientists have recently focused on conceiving new ways for treating infections with a longer duration of action and minimum environmental toxicity. One approach in infection control is based on the development of antimicrobial coatings based on polymers and antimicrobial peptides, also termed as "natural antibiotics".

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

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.

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

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.

Advances in Polymer Based Composite Coatings.

Polymer based composite coatings represent an important class of materials for various applications [...].

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

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.

Multifunctional Hydroxyapatite Coated with Arthemisia absinthium Composites.

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.

Peppermint Essential Oil-Doped Hydroxyapatite Nanoparticles with Antimicrobial Properties.

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.

THE DEVELOPMENT OF A NOVEL ARRAY DETECTOR FOR OVERCOMING THE DOSIMETRY CHALLENGES OF MEASURING IN VERY SHORT PULSED CHARGED PARTICLE BEAMS: THE ELIDOSE PROJECT.

In-beam dose measurements are paramount for any application seeking to harness the effects of the radiation beam, so all the future applications of the laser accelerated beams (as generated in the ELI and CETAL projects) will need such measurements. With a very long history in measuring doses in charged particle beams, the medical and industrial applications setup a number of methods that could be also used for the dosimetry of the beams generated by laser pulses. Dose measurements rely heavily on what is seen as the gold standard in dose measurement: the ion chambers. Ion chambers have both limitations and advantages, and in our case the disadvantage could be the large number of corrections to be applied in order to calculate a correct dose from the measured charge. The ELIDOSE project tries to address these problems by proposing an array detector that would allow the simultaneous measurement of the recombination and polarity corrections, and of the dose. The detector consists of four identical ion chambers mounted together in a PMMA frame and the project will analyze its response to various charged particle beams and the reciprocal influences of the chambers on each other. These reciprocal influences of the four chambers are studied through the FLUKA modeling of the detector and, in order to hone the simulations of the detectors, we initially compared the results of the measurements performed with an Advanced MarkusTM chamber in the proton beam delivered at the 3-MV TandetronTM from IFIN-HH. The paper presents the results of these initial measurements and how these results will be used to modify the simulation parameters.

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

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 (SBET), total pore volume (VP) and pore size (DP) 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.

Morphological and Structural Analysis of Polyaniline and Poly(o-anisidine) Layers Generated in a DC Glow Discharge Plasma by Using an Oblique Angle Electrode Deposition Configuration.

This work is focused on the structural and morphological investigations of polyaniline and poly(o-anisidine) polymers generated in a direct current glow discharge plasma, in the vapors of the monomers, without a buffer gas, using an oblique angle-positioned substrate configuration. By atomic force microscopy and scanning electron microscopy we identified the formation of worm-like interlinked structures on the surface of the polyaniline layers, the layers being compact in the bulk. The poly(o-anisidine) layers are flat with no kind of structures on their surfaces. By Fourier transform infrared spectroscopy we identified the main IR bands characteristic of polyaniline and poly(o-anisidine), confirming that the polyaniline chemical structure is in the emeraldine form. The IR band from 1070 cm-1 was attributed to the emeraldine salt form of polyaniline as an indication of its doping with H⁺. The appearance of the IR band at 1155 cm-1 also indicates the conducting protonated of polyaniline. The X-ray diffraction revealed the formation of crystalline domains embedded in an amorphous matrix within the polyaniline layers. The interchain separation length of 3.59 Šis also an indicator of the conductive character of the polymers. The X-ray diffraction pattern of poly(o-anisidine) highlights the semi-crystalline nature of the layers. The electrical conductivities of polyaniline and poly(o-anisidine) layers and their dependence with temperature are also investigated.

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

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.

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

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 xAg = 0 (HAp) and xAg = 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.