The sorption of lead by synthetic hydroxyapatite (HA) from solutions containing Pb2+ initial concentrations up to 1770 mg L(-1) was studied. X-ray diffractometry (XRD) associated with Rietveld methodology for refining the spectra pattern was used in order to characterize the mechanisms of lead uptake. It is shown that the dissolution of hydroxyapatite is followed by the formation of a solid solution, Pb(10-x)Ca(x)(PO4)6(OH)2, with Pb ions mostly occupying Ca(II) sites. The Ca/Pb molar ratio of this solid solution decreases continuously until it reaches the structure of a pure hydroxypyromorphite. The cell parameters and the crystallite mean size behavior of both mineral phases reinforce the hypothesis that hydroxypyromorphite, PbHA, formation is the end of a process in which Pb(10-x)Ca(x)(PO4)6(OH)2 crystallites are continuously dissolved and recrystallized producing crystals with lower calcium content. Combination of Inductively Coupled Plasma spectrometry (ICP), chemical analysis, and XRD results permitted the conclusion that lead ions are not completely immobilized by precipitating Pb(10-x)Ca(x)(PO4)6(OH)2. Additional surface mechanisms also contribute to Pb2+ uptake. During Pb2+ sorption process, pH variations of the solution phase showed a more complex pattern than previously reported. Contribution of surface mechanisms, in addition to the hydroxyapatite dissolution, could explain this behavior.
Bovine serum albumin (BSA) may have an inhibitory or promoter effect on hydroxyapatite (HA) nucleation when apatite is precipitated in a medium containing the protein. In this study we evaluated the influence of BSA on the precipitation of calcium phosphate phases (CP) from simulated body fluid (SBF) when the protein was previously bounded to HA surface. The kinetics of BSA immobilization onto hydroxyapatite surface was performed in different buffers and protein concentrations in order to adjust experimental conditions in which BSA was tightly linked to HA surface for long periods in SBF solution. It was shown that for BSA concentration higher than 0.1mg/mL the adsorption to HA surface followed Langmuir-Freundlich mechanisms, which confirmed the existence of cooperative protein-protein interactions on HA surface. Fourier Transformed Infrared Attenuated Total Reflectance Microscopy (FTIRM-ATR) evidenced changes in BSA conformational state in favor of less-ordered structure. Analyses from high resolution grazing incident X-ray diffraction using synchrotron radiation (GIXRD), Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) showed that a poorly crystalline calcium phosphate was precipitated on the surface of HA discs coated with BSA, after the immersion in SBF for 4 days. The new bioactive layer had morphological characteristics similar to the one formed on the HA surface without protein. It was identified as a carbonated apatite with preferential crystal growth along apatite 002 direction. The GIXRD results also revealed that BSA layer bound to the surface inhibited the HA dissolution leading to a reduction on the formation of new calcium phosphate phase.
Hydroxyapatite (HA) is capable of accepting substitute ions within its lattice, including zinc ions. Zinc is a trace element that activates the osteogenesis of osteoblastic cells and therefore plays an important role in the activity of alkaline phosphatase enzyme. The purpose of this work was to produce and characterize 5% mol Zn bioceramic in granular form (Zn-granules) for clinical applications and compare it with granules made from HA by using the same production route. Granules with addition of porogen agents were produced from powders of HA and zinc-containing HA by uniaxial pressing and heat treatment. The granules were subsequently ground and sieved. The results indicated that zinc contributed to the reduction of sample crystallinity and formed a biphasic structure after calcination at 1200 °C. Additionally, zinc release from granular material may have clinical applications as bone graft
Poly(lactic-co-glycolic acid) (PLGA) has been used in the field of tissue engineering as a scaffold due to its good biocompatibility, biodegradability and mechanical strength. With the aim to explore the degradability of PLGA electrospun nonwoven structures for oral mucosa tissue engineering applications, non-irradiated and gamma irradiated nonwovens were immersed in three different solutions, in which simulated body fluid (SBF) and artificial saliva are important for future oral mucosa tissue engineering. The nonwovens were immersed for 7, 15 and 30 days in SBF, culture media (DMEM) and artificial saliva at 37 °C. Before immersion in the solutions, the dosage of 15 kGy was applied for sterilization in one assay and compared with non-irradiated samples at the same timepoints. Samples were characterized using different techniques such as scanning electron microscopy (SEM), differential scanning calorimetric (DSC) and gel permeation chromatography (GPC) to evaluate the nonwoven degradation and Fourier-transform infrared spectroscopy (FTIR) to evaluate the chain scissions. Our results showed that PLGA nonwovens were constituted by semicrystalline fibers with moderate degradation properties up to thirty days. The non-irradiated samples exhibited slower kinetics of degradation than irradiated nonwovens. For immersion times longer than 7 days in the three different solutions, the mean diameter of irradiated fibers stayed in the same range, but significantly different from the control sample. On non-irradiated samples, the degradation kinetics was slower and the plateau in the diameter value was only attained after 30 days of immersion in the fluids. Plasticization (fluid absorption into the fiber structure) occurred in the bulk material, as confirmed by a decrease in Tg observed by DSC analyses of non-irradiated and irradiated nonwovens, in comparison with the respective controls. In addition, artificial saliva showed a higher capacity of influencing PLGA crystallization than SBF and DMEM. FTIR analyses showed typical PLGA chemical functional groups changes. These results will be important for future application of those PLGA electrospun nonwovens for oral mucosa regeneration.
Carbonated apatite (CHA) is commonly considered a promising synthetic material for biomedical applications in orthopedic and dental surgery due to its biocompatibility, bioresorption and bioactivity. CHA5, CHA37 and CHA90 powders were synthesized from wet method and the DRX patterns showed that the crystallinity and particle size of CHA samples increased proportionally with the synthesis temperature. Powder extracts medium were obtained from each sample to interact with MC3T3-E1 osteoblastics cells. It was evaluated morphology, citotoxicity, pH and Ca2+ concentration. Citotoxicity assays showed high metabolic activity on all samples when compared to control. The polygonal shaped and the confluent monolayer observed in control cells progressively changed according to the crystallinity increase of samples. Cells under mitosis and spindle-like shaped where the main alterations observed. In addition the cell viability could be sensitive to the acid reactivity and crystallinity of carbonated apatite samples.
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