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Bioactive hydroxyapatite (HA) coating on titanium (Ti) implant can be used as a drug delivery device. A controlled release of drug around the implant requires the incorporation of drug into the coating material during the coating process. HA coating was prepared using a two-step procedure in conditions suitable for simultaneous incorporation of the protein-based drug into the coating material. Monetite coating was deposited on Ti substrate in acidic condition followed by the transformation of the monetite coating to HA. X-ray diffraction (XRD) confirmed the formation of the monetite phase at the first step of the coating preparation, which was transformed into HA at the second step. Fourier transform infrared spectroscopy demonstrated typical bands of a crystallized carbonated HA with A- and B-type substitution, which was confirmed by the XRD refinement of the structural parameters. Scanning electron microscope was used to observe the morphology of monetite and HA coatings. Adhesion of the coatings was measured using a scratch tester. The critical shearing stress was found to be 84.20 ± 1.27 MPa for the monetite coating, and 44.40 ± 2.39 MPa for the HA coating.

Tricalcium phosphate (TCP) is recognized as a promising bone replacement material due to its high bioactivity and resorbable properties. To mimic biological apatites, incorporation of magnesium (Mg) in TCP was proposed. Mg-substituted TCP (beta-TCMP) and beta-TCP dense tablets were obtained by pressing and sintering at 1,000 degrees C Mg-substituted calcium deficient apatite (Mg-CDA) and commercial TCP, respectively. The materials were characterized using X-ray diffraction, infrared spectroscopy and electron microscopy. Human osteoblast cells (SaOs2) were seeded onto the sintered tablets for 4 h, 24 h and 7 days. Results showed that Mg-CDA was completely transformed into beta-TCMP. Moreover, beta-TCMP stimulated adhesion and proliferation of human osteoblast cells. Consequently, the magnesium incorporation on calcium deficient apatites followed by sintering at 1,000 degrees C seems to be a useful path to obtain biocompatible and non cytotoxic dense tablets with TCP structure with potential application on bone engineering.

Fluoride (F-)-substituted B-type carbonate hydroxyapatite (CHAP) powders were prepared for application as bone substitute materials having the ability to enhance bone formation and to suppress bone resorption due to the therapeutic effect of F-. F- was adsorbed on CHAP in a sodium fluoride solution followed by heating at 700 degrees C in carbon dioxide flow to substitute F- for the hydroxyl ion in the CHAP structure. The F- contents in the F-substituted CHAP powders were 16-22 times greater than that in normal adult human bones. The carbonate ion contents in the F-substituted CHAP powders corresponded to or were higher than that in normal adult human bones. F-substituted CHAP powder with CO3(2-) and F- contents of 11.03 and 0.66 wt%, respectively, slowly released F- in a physiological salt solution to a sufficiently high F- level. The F- concentration slowly increased and reached 67.20 +/- 4.81 microg l(-1), which was 1.5-9.3 times higher than that in the body fluid of normal adult humans, near the therapeutic window of F-, and far lower than the estimated toxic level. Therefore, the F-substituted CHAP can promote bone formation. The present F-substituted CHAP has the advantage of slow F- release over sodium fluoride and sodium monofluorophosphate which are highly soluble salts and cannot be sintered into a ceramic body.

The purpose of this study was to investigate the bone regenerative effect of calcium phosphate glass in vivo. We prepared two different sizes of calcium phosphate glass powder using the system CaO-CaF2-P2O5-MgO-ZnO; the particle size of the powders were 400 microm and 40 microm. 8 mm calvarial critical-sized defects were created in 60 male Sprague-Dawley rats. The animals were divided into 3 groups of 20 animals each. Each defect was filled with a constant weight of 0.5 g calcium phosphate glass powder mixed with saline. As controls, the defect was left empty. The rats were sacrificed 2 or 8 weeks after postsurgery, and the results were evaluated using radiodensitometric and histological studies; they were also examined histomorphometrically. When the bigger powders with 400 microm particle were grafted, the defects were nearly completely filled with new-formed bone in a clean healing condition after 8 week. When smaller powders with 40 microm particle were transplanted, new bone formation was even lower than the control group due to a lot of inflammatory cell infiltration. It was concluded that the prepared calcium phosphate glass enhanced the new bone formation in the calvarial defect of Sprague-Dawley rats and it is expected to be a good potential materials for hard tissue regeneration. The particle size of the calcium phosphate was crucial; 400 microm particles promoted new bone formation, while 40 microm particles inhibited it because of severe inflammation.

The influence of temperature and aging time on the morphology and mechanical properties of nano-sized hydroxyapatite (HA) synthesized by a hydrothermal method is reported here. The pre-mixed reactants were poured into a stirred autoclave and reacted at temperatures between 25-250 degrees C for 2-10 h. HA powders thus obtained were examined using X-ray diffraction (XRD), high-resolution field emission scanning electron microscopy (FESEM) and a particle size analyzer. It was found that the aspect ratio of the particles increased with the reaction temperature. The length of the HA particles increased with the reaction temperature below 170 degrees C, but it decreased when the temperature was raised above 170 degrees C. The agglomerates of HA particles were formed during synthesis, and their sizes were strongly dependent on reaction temperatures. As the reaction temperature increased, the agglomerate size decreased (p = 0.008). The density of the discs pressed from these samples reached 85-90% of the theoretical density after sintering at 1200 degrees C for 1 h. No decomposition to other calcium phosphates was detected at this sintering temperature. A correlation existed (p = 0.05) between the agglomerate sizes of HA particles synthesized at various conditions and their sintered densities. With the increase of the agglomerate size, the sintered density of the HA compact decreased. It was found that both the sintered density and flexural strength increased with increasing aging time and reaction temperature. A maximum flexural strength of 78 MPa was observed for the samples synthesized at 170 degrees C for 5 h with the predicted average at these conditions being 65 MPa. These samples attained an average sintered density of 88%.

Biphasic calcium phosphate (BCP) bioceramics belong to a group of bone substitute biomaterials that consist of an intimate mixture of hydroxyapatite (HA), Ca(10)(PO(4))(6)(OH)(2), and beta-tricalcium phosphate (beta-TCP), Ca(3)(PO(4))(2), of varying HA/beta-TCP ratios. BCP is obtained when a synthetic or biologic calcium-deficient apatite is sintered at temperatures at and above 700 degrees C. Calcium deficiency depends on the method of preparation (precipitation, hydrolysis or mechanical mixture) including reaction pH and temperature. The HA/beta-TCP ratio is determined by the calcium deficiency of the unsintered apatite (the higher the deficiency, the lower the ratio) and the sintering temperature. Properties of BCP bioceramics relating to their medical applications include: macroporosity, microporosity, compressive strength, bioreactivity (associated with formation of carbonate hydroxyapatite on ceramic surfaces in vitro and in vivo), dissolution, and osteoconductivity. Due to the preferential dissolution of the beta-TCP component, the bioreactivity is inversely proportional to the HA/beta-TCP ratio. Hence, the bioreactivity of BCP bioceramics can be controlled by manipulating the composition (HA/beta-TCP ratio) and/or the crystallinity of the BCP. Currently, BCP bioceramics is recommended for use as an alternative or additive to autogeneous bone for orthopedic and dental applications. It is available in the form of particulates, blocks, customized designs for specific applications and as an injectible biomaterial in a polymer carrier. BCP ceramic can be used also as grit-blasting abrasive for grit-blasting to modify implant substrate surfaces. Exploratory studies demonstrate the potential uses of BCP ceramic as scaffold for tissue engineering, drug delivery system and carrier of growth factors.

Two different preparations of biphasic calcium phosphate (BCP) were characterized in vitro: BCP1 from a mechanical mixture of hydroxyapatite (HA) and beta-tricalcium phosphate (beta-TCP) powders, and BCP2 from calcination of a calcium-deficient apatite (CDA). The structural, physicochemical and mechanical parameters of these two preparations were investigated, and two different macroporous BCP1 (MBCP1) and BCP2 MBCP2) implants were manufactured and implanted in rabbit bone for in vivo bioactivity studies. Scanning electron microscopy observations showed that MBCP1 implants had a significantly higher degradation rate (P<0.0001) than MBCP2 implants. This was probably caused by the presence of calcium oxide impurities in BCP1 and the more intimate mixture and stable ultrastructure of BCP2. No significant difference about the newly formed bone rate in these two BCP preparations was observed. Very slight variations in sintering conditions appeared to influence the biodegradation behavior of the two MBCP implants despite their identical HA/-TCP ratios and similar porosity. Precise and complete in vitro characterization enabled us to understand and predict in vivo degradation behavior.

A new injectable biomaterial for bone and dental surgery is a composite consisting of a polymer as a matrix and bioactive calcium phosphate (CaP) ceramics as fillers. The stability of the polymer is essential in the production of a ready-to-use injectable sterilized biomaterial. The purpose of this study was to detect possible polymer degradation which may have been caused by the interaction with the fillers using Fourier transform infrared spectroscopy. Composites containing CaP fillers (biphasic calcium phosphate, hydroxyapatite and peroxidized hydroxyapatite) and polymer (hydroxypropyl methyl cellulose) were prepared. To investigate the properties of the polymer, the inorganic and organic phases of the composite were separated using several extraction methods. The difficulty in separating the organic (polymer) from the mineral (CaP fillers) phases in the composite investigated in this study suggested the presence of strong interactions between the two phases. Spectra of extracted polymers showed new absorption bands of low intensities and indications that some chemical modifications of the original polymers have occurred. Results also indicated that the filler composition has an effect on the integrity of the polymer.