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PubMed2004

Photoexcited formation of bone apatite-like coatings on micro-arc oxidized titanium.

A novel method to rapidly deposit bone apatite-like coatings on titanium implants in simulated body fluid (SBF) is proposed in this article. The processing was composed of two steps; for example, micro-arc oxidation (MAO) of titanium to form titania films, and UV-light illumination of the titania-coated titanium in SBF. The morphology, crystalline structure, and bond strength of the MAO films were investigated as a function of the applied voltage (in the range of 250-400 V) by using scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectrometry, Fourier transform infrared spectroscopy, adhesion-tensile test, and scratch test. Results showed that the MAO films were porous and nanocrystalline with pore sizes varying from 1 to 3 microm and grain sizes varying from 10-20 to 70-80 nm; the predominant phase in titania films changed from anatase to rutile, and the bond strength of the films decreased from 43.4 to 32.9 MPa as the applied voltage increased from 250 to 400 V. After UV-light illumination of the films in SBF for 2 h, bone apatite-like coating was deposited on the MAO film formed at 250 V. The bond strength of the apatite/titania bilayer was about 44.2 MPa. However, no apatite was observed on the MAO film formed at 400 V after UV-light illumination.

Apatites↗

PubMed2005

Early apatite deposition and osteoblast growth on plasma-sprayed dicalcium silicate coating.

Dicalcium silicate coating was deposited onto a Ti-6Al-4V substrate using plasma-spraying technology. The coating was immersed in simulated body fluid (SBF) for 1, 3, 6, 12, 24, and 48 h to investigate early apatite formation on the coating. Osteoblasts were also seeded onto the surface of the dicalcium silicate coating to evaluate its biocompatibility. Cold field-emission scanning electron microscopy and energy-dispersive X-ray spectrometry were used to evaluate the morphologies and determine the chemical composition of the coatings. The surface structural changes caused by immersion in SBF were analyzed using thin-film X-ray diffraction. After the dicalcium silicate coating was soaked in SBF solution 1-6 h, two types of particles containing calcium and phosphorus were formed on the surface. One type consisted of relatively larger particles (P1) precipitated on the surface of the coating from the precursor cluster formed in the SBF solution. The second type was composed of particles (P2) nucleated on the surface of the coating. With increasing immersion time, the particles coalesced to form a surface Ca-P layer. The Ca-P layer was composed of amorphous calcium phosphate that was not transformed to crystalline apatite until the immersion time in SBF exceeded 24 h. The formation mechanism of the Ca-P layer and apatite on the surface of the coating is believed to be involved in the formation of the Si 3-ring active surface site with negative charge. The cell-seeding test revealed that osteoblasts grew and proliferated very well on the surface of the dicalcium silicate coating.

Animals↗

PubMed2006

Directional/acidic dissolution kinetics of (OH,F,Cl)-bearing apatite.

Directional dissolution of a natural (OH,F,Cl)-bearing apatite has been studied at various solution pH values (0-3) and 30 degrees C. This apatite showed abnormally high O--H stretching frequencies due to the substitution of Cl for OH. The advance of dissolution front indicated that steady-state directional dissolution for pH = 0-2 followed an apparent rate law of Rate = ka(H+) (n) (in mole/m(2)h), where the rate constants (k) are 2.15 and 1.61; and the rate orders (n) are 1.44 and 1.30 for [0001] and <1,120> directions, respectively. Previous study, however, indicated a smaller n value (n = 0.55-0.70) for fluorapatite powders at higher pHs. A nonlinear pH dependence of logarithmic dissolution rate at a wide pH range implied that the surface active sites and/or rate-determining steps have changed when the acidity of solution and/or the composition of the apatite were changed. The opening of etch pits on basal planes further indicated that the dissolution rates along the three principal directions have the following relationship: [0001] > <1,120> > <1,010> for pH=0-1, but the order was reversed for pH > 3.

Acids↗

PubMed2004

Apatite formation on the surface of wollastonite/tricalcium phosphate composite immersed in simulated body fluid.

Wollastonite/tricalcium phosphate composites were prepared and immersed in SBF for various periods to investigate the apatite-formation mechanism on their surfaces. Surface morphologies and composition before and after immersion were analyzed by SEM and EDS technologies. The concentration changes of calcium, silicon, and phosphorus in SBF due to the immersion of the samples were measured with inductively coupled plasma atomic emission spectroscopy, and the corresponding pH values in SBF were recorded. XRD and IR were used to examine the changes in crystalline phases and functional groups. It was found that, after immersion for 1 day, the samples were covered by pom-pom-like apatite granules, resulting from the dissolution of wollastonite and the simultaneous transformation of TCP. This quickly led to the subsequent precipitation of another apatite layer, which covered the earlier-formed surface completely. These results indicate that the wollastonite/tricalcium phosphate composite is a potential biomaterial candidate because of its high bioactivity and in situ porous structure.

Apatites↗

PubMed2006

Composite coating of bonelike apatite particles and collagen fibers on poly L-lactic acid formed through an accelerated biomimetic coprecipitation process.

Collagen and apatite were coprecipitated as a composite coating on poly L-lactic acid (PLLA) in an accelerated biomimetic process. The incubation solution contained collagen (1 g/L) and simulated body fluid with 5 times inorganic ionic concentrations as human blood plasma. The coating formed on PLLA films and scaffolds after a 24-h incubation was characterized by using energy-dispersive X-ray spectroscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy (SEM). It was shown that the coating contained carbonated bonelike apatite and collagen, which was similar in composition to natural bone. SEM showed a complex composite coating of submicron bonelike apatite particulates combined with collagen fibrils. It is expected that such biocomposite coating may better facilitate cell interaction and osteoconductivity. This work provided an efficient process to obtain bonelike apatite/collagen composite coating, which is potentially useful in bone tissue engineering.

Apatites↗

PubMed1999

Intravertebral body reconstruction with an injectable in situ-setting carbonated apatite: biomechanical evaluation of a minimally invasive technique.

The ability to mechanically reinforce an osteoporotic vertebral body could impede spinal compression fracture and the associated pain and complications. Previous studies have shown that reinforcement of fractured vertebrae with conventional acrylic cement can relieve symptoms and avoid further collapse. In this study, we explored the use of a carbonated apatite cement combined with a minimally invasive injection technique to improve the compressive mechanical properties of cadaveric vertebral bodies. After establishing the biomechanical characteristics of cement formulations intended to have appropriate viscosities, we evaluated the infiltration of the cements into thoracic vertebral bodies using a combined suction-injection technique. The energy-absorption capabilities of the reinforced vertebral bodies were then measured during axial compressive tests and compared with those of nonreinforced vertebrae. The ultimate compressive strength of the cement formulations averaged from 11.6 to 17.7 MPa, depending on curing conditions. The suction-injection technique allowed from one-half to two-thirds of each vertebral body to be infiltrated with cement. Energy absorption was significantly higher (p < 0.05) between 25 and 70% collapse of the vertebral body in the specimens that received the apatite injection as compared with the controls. These results suggest that osteoporotic vertebral-body augmentation with the injection of apatite cement could prevent further collapse after initial failure has occurred. The osteoconductive nature of the cement and its ability to be remodeled by bone, together with its compressive strength, which is higher than that of cancellous bone, could provide better clinical results than those of current treatments with acrylic cement.

Aged↗

PubMed1992

Competitive adsorption of magnesium and calcium ions onto synthetic and biological apatites.

Magnesium (Mg) is a conspicuous constituent of hard tissues but its possible role in biomineralization is poorly understood. It is possible that Mg2+ adsorbed onto bioapatites may contribute to the modulation of crystal growth as such inhibitory activity has been reported for synthetic apatites. The present study was undertaken to determine the adsorption isotherms of Mg ions onto synthetic apatites and biominerals in tooth and bone tissues in the presence of other ions of natural occurrence. Synthetic crystals used as adsorbents were hydroxyapatite and, as a better prototype for the biomineral, Mg-containing carbonatoapatite. Human enamel and dentin materials were obtained from extracted, caries-free, permanent teeth. Porcine dentin materials at two developmental stages were obtained from erupted deciduous and unerupted permanent teeth of a 6-month-old slaughtered piglet. Porcine bone was obtained from the cortical portion of the mandible of the same animal. All biomineral samples were pulverized and then treated by plasma ashing (deproteination) at about 60 degrees C. Each of the powdered samples was equilibrated in solutions containing various initial concentrations of Mg2+, Ca2+, and Na+ (or K+) as nitrate salts. Following equilibration, concentrations (and activities) of magnesium and calcium ions in the experimental solution were determined. The pH values of the equilibrium solutions were in the range of 6.2-6.5. Experimental data of the Mg adsorption onto hydroxyapatite were interpreted on the basis of a Langmuir-type model for binary systems assuming competition of Mg2+ and Ca2+ for the same adsorption sites on the crystal surfaces of the apatites.(ABSTRACT TRUNCATED AT 250 WORDS)

Adsorption↗

PubMed1994

Bioactive glass-ceramic containing crystalline apatite and wollastonite initiates biomineralization in bone cell cultures.

Rat bone cells were cultured in the presence of bioactive glass-ceramic containing crystalline apatite and wollastonite. Scanning electron microscopy observations of the surface of the seeded ceramic disks revealed that cells attached, spread, and proliferated on the material surface. Soaking in cell-free culture medium showed that no change occurred in the surface structure. However, when cultured with bone cells and observed under a transmission electron microscope, an electron-dense layer was noted initially at the surface of the material, before bone formation occurred. In addition, energy-dispersive X-ray microanalysis demonstrated the presence of calcium and phosphorus in this layer. Progressively, during the following days of culture, active osteoblasts synthetized and laid down an osteoid matrix composed of numerous collagen fibrils arranged either parallel or perpendicularly to the first-formed electron-dense layer. Mineralization initiated on the ceramic surface dispersed then along the collagenous fibrils, leading to a mineralized matrix which surrounded the ceramic particles. These results demonstrate the capacity of apatite-wollastonite glass ceramic to initiate biomineralization in osteoblast cultures and to achieve a direct bond between the surface apatite layer of the bioactive glass-ceramic and the mineralized bone matrix.

Animals↗

PubMed1993

Epitaxial overgrowth of apatite crystals on the thin-ribbon precursor at early stages of porcine enamel mineralization.

The aim of the present work was to investigate changes in cross-sectional morphologies of enamel crystallites as a function of location in secretory porcine enamel. Enamel tissues were obtained from 5- to 6-month-old slaughtered piglets. For examination by electron microscopy, a portion of the secretory enamel was embedded in resin and ultrathin sections were prepared with a diamond knife. In parallel studies, compositional and structural changes of enamel mineral were assessed by chemical analysis and Fourier transform infrared (FTIR) spectroscopy. For this purpose, two consecutive layers of the outer secretory enamel, each approximately 30 microns thick, were separated from the labial side of permanent incisors. Using high-resolution electron microscopy, early events of enamel crystal growth were characterized as the epitaxial growth of small apatite units on the lateral surfaces of the initially precipitated thin ribbon. These apatite units had regular triangle or trapezoid cross-sections. After fusions of those isolated trapezoids on both lateral sides of the platy template, the resulting enamel crystallites had the well-documented flattened-hexagonal shapes in cross-sections. The initially precipitated thin plate was buried inside the overgrown apatite lamella and then retained as a central dark line. Similar morphological evidence for the epitaxial nucleation and overgrowth of carbonatoapatite on the platy template was obtained in vitro. Chemical and FTIR analyses of the enamel layer samples showed that the characteristics of the youngest enamel mineral were distinct from those of enamel crystals found in older secretory enamel.(ABSTRACT TRUNCATED AT 250 WORDS)

Animals↗

PubMed1989

Osteoarthrosis and apatite synovitis. Pathological study of a metacarpophalangeal joint.

A case of metacarpophalangeal osteoarthrosis associated with synovial apatite deposits is reported. The size of the crystals indicates that they have been thickened by a recrystallization process; the latter could have been provoked by Ca and Po4 ions released by dissolution of some apatite crystals brought by calcified debris of bone or cartilage coming from the abraded osteoarthrotic surfaces. The role of such thickened crystals in synovial inflammation is discussed as well as their possible diagnostic value in determining origin and pathogenesis of a given synovial apatite deposit.

Apatites↗

PubMed1980

A mechanism for incorporation of carbonate into apatite.

Octacalcium phosphate (Ca8H2(PO4)6 . 5H2O) is considered to be precursor in the formation of apatite in bones and teeth; a crucial step for incorporation of impurities appears to occur during its hydrolysis. The present study examines the role that octacalcium phosphate plays in the process of incorporation of carbonate into apatite. Chemical, X-ray diffraction, and infrared techniques were used. When octacalcium phosphate is hydrolyzed in the presence of sodium and carbonate ions in aqueous media, approximately one sodium and one carbonate ion seem to substitute for a calcium and phosphate ion, respectively, in forming apatite, and the a axis is shortened. The infrared spectrum of the product indicates that the carbonate is in the type B site, which is presumed to be a phosphate site. This mechanism is of particular importance since the presence of carbonate in human enamel appears to be related to caries susceptibility. A structural mechanism for the incorporation of impurities during hydrolysis of octacalcium phosphate is presented.

Apatites↗

PubMed1979

Composition of apatites in human urinary calculi.

Calcium-deficient carbonate apatites in urinary calculi from 17 patients have been studied. Magnesium ions in each case were detected as a component of apatite. In most of the cases, CO23- ions were included in the apatitic lattice. Using a calcination procedure, we have determined the most probable average value for the CO23- content, degree of deficiency, x, and the Mg/Ca ratio in each sample.

Apatites↗

PubMed1986

Water on apatites.

Adsorption of water was studied gravimetrically at 23 degrees C in an open system at several relative humidities on a variety of apatitic calcium phosphates including enamel, deproteinized enamel, and bone mineral. The amount of adsorbed water increases linearly with the surface areas of the synthetic apatites and does not appear very sensitive to calcium to phosphorus ratio of the apatites. The adsorption results correlate very well up to about two monolayers with a conventionally determined isotherm. Higher uptake of water even by "deproteinized" enamel or bone may be due to the presence of pore structure and incompletely removed organic matter.

Adsorption↗

PubMed1991

Solid state 31NMR studies of the conversion of amorphous tricalcium phosphate to apatitic tricalcium phosphate.

The hydrolytic conversion of a solid amorphous calcium phosphate of empirical formula Ca9 (PO4)6 to a poorly crystalline apatitic phase, under conditions where Ca2+ and PO4(3-) were conserved, was studied by means of solid-state magic-angle sample spinning 31P-NMR (nuclear magnetic resonance). Results showed a gradual decrease in hydrated amorphous calcium phosphate and the formation of two new PO4(3-)-containing components: an apatitic component similar to poorly crystalline hydroxyapatite and a protonated PO4(3-), probably HPO4(2-) in a dicalcium phosphate dihydrate (DCPD) brushite-like configuration. This latter component resembles the brushite-like HPO4(2-) component previously observed by 31P-NMR in apatitic calcium phosphates of biological origin. Results were consistent with previous studies by Heughebaert and Montel [18] of the kinetics of the conversion of amorphous calcium phosphate to hydroxyapatite under the same conditions.

Apatites↗

PubMed1991

A correlation between the distribution of biological apatite and amino acid sequence of type I collagen.

We have determined the localization of apatite within type I collagen fibrils of calcifying turkey leg tendons by both bright field and selected-area dark field (SADF) electron microscopy and have compared this to computer-modeled, chick type I collagen amino acid sequence data. Apatite crystals occur in both the gap and overlap zones at early stages of mineralization in an asymmetric pattern that corresponds to the polarity, N- to C- orientation, of the collagen molecule. Based on comparisons with computer-generated models of known amino acid sequence of collagen, it was determined for early stages of mineral deposition that apatite is restricted by areas of high hydrophobicity. The gap zone is less hydrophobic than the overlap zone on average but each of these zones had areas of high hydrophobicity that correlated with sites of low localization of mineral. Possible interactions between hydrophobic regions and the process of mineral deposition are discussed.

Amino Acid Sequence↗

PubMed2000

Fourier transform infrared determination of CO2 evolved from carbonate in carbonated apatites.

A quantitative method based on FTIR has been developed to determine carbonate in synthetic apatites. The method measures the evolved CO2 after reaction of 50 mg apatite with 2 mL of hydrochloric acid (0.5 M) in a reaction vessel, heated to 40 degrees C. The CO2 evolved was swept by a carrier of nitrogen to a laboratory-made infrared gas cell of 39 mm pathlength and 490 microL volume. The signals were recorded as a function of time and the areas of the chemigram peaks obtained from the measurements in the wavenumber range of 2,500-2,150 cm(-1), were interpolated using a calibration curve. The method can be used to study apatites with carbonate contents below 0.2% with a sampling frequency of 8 h(-1).

Apatites↗

PubMed1998

The effect of fluoride on the size and morphology of apatite crystals grown from physiologic solutions.

In adult human bone, fluoride uptake is accompanied by an increase in apatite crystal size. This increase, however, is not isotropic but is restricted primarily to growth in width and/or thickness, with no measurable change in length. In the present study, seeded growth experiments were conducted in vitro to determine whether this anisotropic effect is physicochemical in origin, i.e., a direct result of F- selectively enhancing lateral crystal growth, or is an indirect consequence of F--induced alterations in cellular function and matrix development. The growth reactions were maintained at 37 degrees C under physiologic-like solution conditions (1.33 mmol/liter Ca2+, 1.0 mmol/liter total phosphate, 0 or 26 mmol/liter carbonate, 270 mmol/kg osmolality, pH 7.4) using constant-composition methods. When new accretions accumulated to three times the initial seed mass, the solids were collected and net crystal growth was assessed by X-ray diffraction line broadening analysis. The X-ray results revealed that the carbonate constituent in our physiologic-like solutions promoted the proliferation of new crystals at the expense of further growth of the seed apatite. Solution F- concentrations of approximately 2 micromol/liter partially offset the repressive effect that carbonate had on primary crystal growth. Moreover, F- stimulated seed crystal growth in the same anisotropic manner as had been observed for adult human bone apatite, a finding that suggests that the latter growth in vivo was the consequence, in part, of direct F--mineral interactions.

Apatites↗

PubMed2004

Ectomycorrhizal fungal biomass in roots and uptake of P from apatite by Pinus sylvestris seedlings growing in forest soil with and without wood ash amendment.

Forest soil from an experimental Norway spruce forest with four levels of wood ash addition (0, 1, 3 and 6 tonnes ha(-1)) was used to inoculate pine (Pinus sylvestris) seedlings with indigenous ectomycorrhizal (EM) fungi. Uptake of 32P and 86Rb in a root bioassay was used to estimate the demand for P and K by seedlings grown in the different soils. Utilisation of P from apatite was tested in a laboratory system where uptake by the ectomycorrhizal mycelium was separated from uptake by roots. The demand for P and K in the seedlings was similar regardless of the ash treatment. Variation in EM levels, estimated as fungal biomass (ergosterol) in roots, was large in the different soils, but not related to ash addition. Uptake of P from apatite was, on average, 23% of total seedling P and was not related to EM levels. It was concluded that the improved P uptake from apatite by EM fungi found in earlier studies is probably not a general phenomenon among EM fungi. The small effect of ash addition on EM levels and P uptake suggests that addition of granulated wood ash is a forest management treatment that will have only minor influence on ectomycorrhizal symbiosis.

Apatites↗