3D Printable Composite Biomaterials Based on GelMA and Hydroxyapatite Powders Doped with Cerium Ions for Bone Tissue Regeneration.

The main objective was to produce 3D printable hydrogels based on GelMA and hydroxyapatite doped with cerium ions with potential application in bone regeneration. The first part of the study regards the substitution of Ca2+ ions from hydroxyapatite structure with cerium ions (Ca10-xCex(PO4)6(OH)2, xCe = 0.1, 0.3, 0.5). The second part followed the selection of the optimal concentration of HAp doped, which will ensure GelMA-based scaffolds with good biocompatibility, viability and cell proliferation. The third part aimed to select the optimal concentrations of GelMA for the 3D printing process (20%, 30% and 35%). In vitro biological assessment presented the highest level of cell viability and proliferation potency of GelMA-HC5 composites, along with a low cytotoxic potential, highlighting the beneficial effects of cerium on cell growth, also supported by Live/Dead results. According to the 3D printing experiments, the 30% GelMA enriched with HC5 was able to generate 3D scaffolds with high structural integrity and homogeneity, showing the highest suitability for the 3D printing process. The osteogenic differentiation experiments confirmed the ability of 30% GelMA-3% HC5 scaffold to support and efficiently maintain the osteogenesis process. Based on the results, 30% GelMA-3% HC5 3D printed scaffolds could be considered as biomaterials with suitable characteristics for application in bone tissue engineering.

Influence of Thermal Treatment Conditions on the Properties of Dental Silicate Cements.

In this study the sol-gel process was used to synthesize a precursor mixture for the preparation of silicate cement, also called mineral trioxide aggregate (MTA) cement. This mixture was thermally treated under two different conditions (1400 °C/2 h and 1450 °C/3 h) followed by rapid cooling in air. The resulted material (clinker) was ground for one hour in a laboratory planetary mill (v = 150 rot/min), in order to obtain the MTA cements. The setting time and mechanical properties, in vitro induction of apatite formation by soaking in simulated body fluid (SBF) and cytocompatibility of the MTA cements were assessed in this study. The hardening processes, nature of the reaction products and the microstructural characteristics were also investigated. The anhydrous and hydrated cements were characterized by different techniques e.g., X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR) and thermal analysis (DTA-DTG-TG). The setting time of the MTA cement obtained by thermal treatment at 1400 °C/2 h (MTA1) was 55 min and 15 min for the MTA cement obtained at 1450 °C/3 h (MTA2). The compressive strength values were 18.5 MPa (MTA1) and 22.9 MPa (MTA2). Both MTA cements showed good bioactivity (assessed by an in vitro test), good cytocompatibility and stimulatory effect on the proliferation of cells.

Collagen/hydroxyapatite composite materials with desired ceramic properties.

Our purpose was to obtain and characterize some collagen/hydroxyapatite (COLL/HA) hybrid composite materials with desired ceramic properties. The ceramic properties of these materials were achieved by combining two drying methods: controlled air drying at 30°C followed by freeze-drying. Through the function of the air drying times, the materials morphology varies from porous materials (when the materials are freeze-dried) up to dense materials (when the materials are air-dried), while the combined drying allows us to obtain an intermediary morphology. The composite materials intended to be used as bone grafts and in a drug delivery system were characterized by XRD, FTIR, SEM, and also by determining the ceramic properties by using the Arthur method. The ceramic properties of these COLL/HA composite materials vary in large range, for instance the density of the materials varies from 0.06 up to 1.5 g/cm(3) while the porosity varies from 96.5% down to 27.5%.

Mineralogical and Microstructural Characteristics of Two Dental Pulp Capping Materials.

This paper aims to investigate the composition, surface, and microstructural characteristics, and bioactivity of two commercially available pulp capping materials known as TheraCal LC and BIO MTA+. The materials were prepared as cylindrical samples and assessed by X-ray diffraction (XRD) and complex thermal analysis for mineralogical characterization, and by scanning electron microscopy (SEM) coupled with energy dispersive of X-ray (EDX), Fourier-Transformed Infrared Spectroscopy (FT-IR), and atomic force microscopy (AFM) for microstructural and surface characteristics. The in vitro bioactivity was highlighted by surface mineralization throughout SEM coupled with EDX and FT-IR analysis. XRD analysis performed on both materials showed calcium silicate phases and different radiopacifying compounds. AFM measurements indicated a smoother and more homogenous surface with a lower average roughness for TheraCal LC due to the resin matrix from its composition. FT-IR analysis displayed bands for several compounds in both materials. Both materials exhibited bioactive properties showing surface mineralization after being immersed in solution similar to the human physiological environment. However, the MTA cement showed a better mineralization due to the anhydrous and hydrated phases.

The effect of dental pulp-capping materials on hard-tissue barrier formation: A systematic review and meta-analysis.

BACKGROUND: The authors of this systematic review aimed to compare the effects of pulp-capping materials on hard-tissue barrier formation using histologic assessments. TYPE OF STUDIES REVIEWED: The authors included randomized controlled trials and controlled clinical trials in humans, with vital therapies performed on healthy permanent teeth undergoing experimental mechanical pulp exposures. They searched electronically in the PubMed, Cochrane, Embase, and Summon databases and carried out a manual search. Twenty-seven full-text articles were eligible for inclusion in the systematic review. After data extraction, the authors performed 2 sets of meta-analyses with odds ratios (OR) and their 95% confidence intervals (CI) on 22 studies. Ten studies compared mineral trioxide aggregate (MTA) with calcium hydroxide (CH), and 12 compared bonding agents with CH. The authors assessed bias by means of Cochrane Collaboration's tool for assessing risk, funnel plots, and Harbord test. RESULTS: The use of MTA was associated with a higher rate of hard-tissue barrier formation than CH. The OR comparing the 2 groups was 2.45 (95% CI, 1.39 to 4.29; P = .002). Use of bonding agents was associated with a lower rate of hard-tissue barrier formation than CH. The OR comparing the 2 groups was 0.02 (95% CI, 0.01 to 0.05; P < .001). CONCLUSIONS AND PRACTICAL IMPLICATIONS: The results suggest that MTA and CH have positive effects on hard-tissue barrier formation. On the basis of the evidence, the authors conclude that MTA has better effects than CH regarding dental pulp protection in the capping of mechanical pulp exposures. Conversely, bonding agents are inferior to CH.

Improvement of silicate cement properties with bacterial cellulose powder addition for applications in dentistry.

The goal of this paper was to synthesize a new family of composites starting from mineral binder powders and biocellulose membranes, with applications in endodontics. An important achievement consisted in the crushing of biocellulose 3D structure in a polygranular powder via an hydrothermal treatment. Afterwards, the polymer powder was mixed with silicate cement powders synthesized through the sol-gel technique. The resulting hybrid materials were investigated by thermal analysis, X-ray diffraction, scanning electron microscopy and mechanical measurements. The hydrocompounds developed after 28days of hardening exhibited an increased structuring degree and favourably adhered to the surface of the embedded biocellulose particles, which led to a faster setting time. A large part of the paper was dedicated to in vitro biological tests. All materials showed a pronounced mineralization process in simulated conditions. Moreover, they did not exert cytotoxic effects, but presented the ability to sustain cell survival and to promote cell proliferation.

Vitroceramic interface deposited on titanium substrate by pulsed laser deposition method.

Pulsed laser deposition (PLD) method was used to obtain biovitroceramic thin film coatings on titanium substrates. The composition of the targets was selected from SiO2-CaO-P2O5-(CaF2) systems and the corresponding masses were prepared using the sol-gel method. The depositions were performed in oxygen atmosphere (100mTorr), while the substrates were heated at 400°C. The PLD deposited films were analysed through different experimental techniques: X-ray diffraction, scanning (SEM, EDX) and transmission (HRTEM, SAED) electron microscopy and infra-red spectroscopy coupled with optical microscopy. They were also biologically tested by in vitro cell culture and the contact angle was determined. The bioevaluation results indicate a high biocompatibilty of the obtained materials, demonstrating their potential use for biomedical applications.

Influence of hot isostatic pressing on ZrO2-CaO dental ceramics properties.

Different hot isostatic pressing conditions were used to obtain zirconia ceramics, in order to assess the influence of HIP on phase transformation, compressive strength, Young's modulus and density. First, CaO stabilized zirconia powder was synthesized through sol-gel method, using zirconium propoxide, calcium isopropoxide and 2-metoxiethanol as precursors, then HIP treatment was applied to obtain final dense ceramics. Ceramics were morphologically and structurally characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Density measurements, compressive strength and Young's modulus tests were also performed in order to evaluate the effect of HIP treatment. The zirconia powders heat treated at 500°C for 2h showed a pure cubic phase with average particle dimension about 70nm. The samples that were hot isostatic pressed presented a mixture of monoclinic-tetragonal or monoclinic-cubic phases, while for pre-sintered samples, cubic zirconia was the single crystalline form. Final dense ceramics were obtained after HIP treatment, with relative density values higher than 94%. ZrO2-CaO ceramics presented high compressive strength, with values in the range of 500-708.9MPa and elastic behavior with Young's modulus between 1739MPa and 4372MPa. Finally zirconia ceramics were tested for biocompatibility allowing the normal development of MG63 cells in vitro.

New Coll-HA/BT composite materials for hard tissue engineering.

The integration of ceramic powders in composite materials for bone scaffolds can improve the osseointegration process. This work was aimed to the synthesis and characterization of new collagen-hydroxyapatite/barium titanate (Coll-HA/BT) composite materials starting from barium titanate (BT) nanopowder, hydroxyapatite (HA) nanopowder and collagen (Coll) gel. BT nanopowder was produced by combining two wet-chemical approaches, sol-gel and hydrothermal methods. The resulting materials were characterized in terms of phase composition and microstructure by X-ray diffraction, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy. Moreover, the biocompatibility and bioactivity of the composite materials were assessed by in vitro tests. The synthesized BT particles exhibit an average size of around 35 nm and a spherical morphology, with a pseudo-cubic or tetragonal symmetry. The diffraction spectra of Coll-HA and Coll-HA/BT composite materials indicate a pronounced interaction between Col and the mineral phases, meaning a good mineralization of Col fibres. As well, the in vitro tests highlight excellent osteoinductive properties for all biological samples, especially for Coll-HA/BT composite materials, fact that can be attributed to the ferromagnetic properties of BT.

Extended release of vitamins from magnetite loaded polyanionic polymeric beads.

Here we explore a novel approach of increasing the release duration of folic and ascorbic acid from magnetite entrapped into calcium-alginate beads. Synthesis and characterization of magnetite-vitamins complexes are reported. The magnetite-vitamins complexes were characterized by FT-IR, XRD, SEM, BET and DTA-TG. Also calcium-alginate magnetic beads were prepared by dripping a mixture of sodium alginate with magnetite-vitamins complexes into calcium chloride solution. Extended release profile of the two experimental models was evaluated and quantified by UV-vis.

Biocompatible hybrid silica nanobiocomposites for the efficient delivery of anti-staphylococcal drugs.

This work reports the non-surfactant templated synthesis and characterization of a new tyrosine-silica/antibiotics (TyR-SiO2/ATBs) nanocomposite, as well as both in vitro and in vivo cytotoxicity and antimicrobial activity against the microbial pathogen Staphylococcus aureus. The in vitro microbiological tests proved that the obtained nanobiostructure significantly enhance the antimicrobial activity of three commonly used antibiotics against S. aureus (i.e. erythromycin (ERI), gentamicin (GEN), and cloxacillin (CLO)) as revealed by the increased diameters of the growth inhibition zones and the decreased minimal inhibitory concentration values, as well as by the inhibitory effect of sub-lethal antibiotic concentrations on the ability of the respective pathogenic strains to adhere and colonize different substrata. These results, correlated with the lack of toxicity against mesenchymal stem cells along with an appropriate in vivo biodistribution highlight the promising therapeutic potential of this carrier that allows a decrease of the required active doses while significantly lessening the harmful side effects of the medication on the host organism.

Biocompatible hydrodispersible magnetite nanoparticles used as antibiotic drug carriers.

Here we report a newly synthesized vectorizing nanosystem, based on hydrodispersible magnetite nanoparticles (HMNPs) with an average size less than 10 nm, obtained by precipitation of Fe(II) and Fe(III) in basic solution of p-aminobenzoic acid (PABA), characterized by high-resolution transmission electron microscopy (HR-TEM), dynamic light scattering (DLS), X-ray diffraction (XRD), differential thermal analysis coupled with thermogravimetric analysis (DTA-TGA) and bioevaluated for cytotoxicity and antibiotic delivery in active forms. The obtained data demonstrate that HMNPs can be used as an efficient drug delivery system, for clinically relevant antimicrobial drugs. HMNPs antimicrobial activity depended on the loaded drug structure and the tested microbial strain, being more efficient against Pseudomonas aeruginosa, comparing with the Escherichia coli strain. The novel HMNPs demonstrated an acceptable biocompatibility level, being thus a very good candidate for biomedical applications, such as drug delivery or targeting.

Plackett-Burman experimental design for bacterial cellulose-silica composites synthesis.

Bacterial cellulose-silica hybrid composites were prepared starting from wet bacterial cellulose (BC) membranes using Stöber reaction. The structure and surface morphology of hybrid composites were examined by FTIR and SEM. The SEM pictures revealed that the silica particles are attached to BC fibrils and are well dispersed in the BC matrix. The influence of silica particles upon BC crystallinity was studied using XRD analysis. Thermogravimetric (TG) analysis showed that the composites are stable up to 300°C. A Plackett-Burman design was applied in order to investigate the influence of process parameters upon silica particle sizes and silica content of BC-silica composites. The statistical model predicted that it is possible for silica particles size to vary the synthesis parameters in order to obtain silica particles deposed on BC membranes in the range from 34.5 to 500 nm, the significant parameters being ammonia concentration, reaction time and temperature. The silica content also varies depending on process parameters, the statistical model predicting that the most influential parameters are water-tetraethoxysilane (TEOS) ratio and reaction temperature. The antimicrobial behavior on Staphylococcus aureus of BC-silica composites functionalized with usnic acid (UA) was also studied, in order to create improved surfaces with antiadherence and anti-biofilm properties.

Silica network improve the effect of fludarabine and paclitaxel on HCT8 cell line.

This paper reports the potential of silica network to sensitize tumor cells and stimulate antitumor toxicity of fludarabine (FLU) and paclitaxel (PAC) against HCT8 cells. SiO2, SiO2/FLU and SiO2/PAC nanostructured materials were characterized by X-Ray Diffraction, Scanning Electron Microscopy, InfraRed Microscopy and in vitro biological assays. When using SiO2/PAC, it can be observed that the cytostatic effect of PAC is boosted only at high concentrations of this material. On the other hand, in the case of SiO2/FLU, data showed an enhancement in the cytostatic activity of FLU by up to 25%, also when using this nanomaterial in low doses. These data represent preliminary study on the impact on silica nano-networks in targeted delivery and controlled release of antitumor drugs and they may be efficiently used for future biomedical applications in cancer therapy.

Synthesis and characterization of COLL-PVA/HA hybrid materials with stratified morphology.

This work presents the synthesis of two hybrid materials: collagen (COLL)-polyvinyl alcohol (PVA) (1:2 wt) and collagen-polyvinyl alcohol/hydroxyapatite (HA) (1:2:3 wt). Starting from the above compositions, different kinds of composites were obtained based on the drying methods: controlled drying at 30°C and freeze drying. The materials were analysed by X-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and scanning electron microscopy (SEM) as well as by measuring the density, porosity and absorption of xylene for each sample by Arthur method. Based on the SEM images, the freeze drying and the controlled drying could be clearly concluded to lead to porous and dense COLL-PVA/HA hybrid materials, respectively. Such materials have exhibited a stratified morphology, the distance between sheets increasing with the increase of the organic components content. Based on the literature data, the obtained COLL-PVA/HA composite materials are valuable bone grafts materials and drug delivery systems.