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PubMedDate not supplied

Differences in solubility of two types of heterogeneous fluoridated hydroxyapatites.

Two types of heterogeneous fluoridated apatites, H-F and F-H, were synthesized by supplying fluoride over the whole range of the degree of fluoridation (X = 0-1.0) during the initial or final half of the experimental period. Although X-ray diffraction patterns and scanning electron microscopy (SEM) photographs of both H-F and F-H type apatites were not significantly different, high-resolution transmission electron microscopy (HR-TEM) showed quite different features; H-F type apatites were elongated hexagons with electron beam damage in the core, while F-H type apatites were rather wider hexagons and approached the typical hexagon of fluorapatite. These results supported the previous speculations on the two different types of heterogeneous fluoridated hydroxyapatites synthesized with fluoride concentration stoichiometrically equivalent to that of fluorapatite: hydroxyapatite covered with fluorapatite and fluorapatite covered with hydroxyapatite. The apparent solubility of H-F type apatites decreased with increases in degree of fluoridation, while that of F-H type apatites decreased markedly and then remained almost constant.

Apatites↗

PubMed2003

Beneficial use of meat and bone meal combustion residue: "an efficient low cost material to remove lead from aqueous effluent".

Meat and bone meal (MBM) combustion residues, a natural apatite-rich substance, was evaluated as a low cost substitute for hydroxyapatite in lead sequestration from water effluents. The thermal behaviour of crude meat and bone meal was followed by TGA and 24% inorganic residue was collected. The resulting ashes were characterised by powder X-ray diffraction (XRD), particle size distribution, specific surface area (BET), and elemental analysis confirming apatite contents, with high level of phosphate (56.3%) and calcium (36.8%). Mechanism and kinetics of lead removal by this bioinorganic material were investigated and compared to mechanisms and kinetics involved with synthetic apatite. Batch metal removal experiments were carried out with 500 and 1500ppm (mg/kg) Pb(2+) solutions. Lead concentration, calcium and pH were monitored. We observed that the mechanism is similar to that occurring for pure apatite, and involved both surface complexation and calcium hydroyapatite (CaHA), Ca(10)(PO(4))(6)(OH)(2), dissolution followed by less soluble Pb(10)(PO(4))(6)(OH)(2) precipitation, as confirmed by XRD analysis of ashes after incubation with lead solution. Our results show that this natural apatite-rich material removes in a few minutes a large quantity of lead (275mg/g capacity) which remains however lower than the theoretical maximum capacity (if calcium were totally substituted by lead). Meat and bone meal combustion residues represent a valuable alternative apatite source for environmental application.

Abattoirs↗

PubMed2000

Reversible suppression of in vitro biomineralization by activation of protein kinase A.

Parathyroid hormone (PTH-(1-34)) potently suppresses apatite deposition in osteoblastic cultures. These inhibitory effects are mediated through signaling events following PTH receptor binding. Using both selective inhibitors and activators of protein kinase A (PKA), this study shows that a transient activation of PKA is sufficient to account for PTH's inhibition of apatite deposition. This inhibition is not a result of reduced cell proliferation, reduced alkaline phosphatase activity, increased collagenase production, or lowering medium pH. Rather, data suggest a functional relationship between matrix assembly and apatite deposition in vitro. Bone sialoprotein (BSP) and apatite co-localize in the extracellular matrix of mineralizing cultures, with matrix deposition of BSP temporally preceding that of apatite. Transient activation of PKA by either PTH-(1-34) or short term cAMP analog treatment blocks the deposition of BSP in the extracellular matrix without a significant reduction in the total amount of BSP synthesized and secreted. This effect is reversible after allowing the cultures to recover in the absence of PKA activators for several days. Thus, a transient activation of PKA may suppress mineral deposition in vitro as a consequence of altering the assembly of an extracellular matrix permissive for apatite formation.

Alkaline Phosphatase↗

PubMed1996

Bonding strength of glass ionomers to dense synthetic hydroxyapatite and fluoroapatite ceramics.

The bonding strength of two glass ionomers, a resin-modified and a conventional one, to dense synthetic hydroxyapatite (HA) and fluoroapatite (FA) ceramics was compared by measuring the shear strength between the ionomers and the apatites. Before the glass ionomers were applied on the apatites, the surfaces of HA and FA plates were either fine-polished or acid-etched after fine polishing. Commercially pure titanium (CP Ti) plates were used as a control. The effects of polyacrylic acid (PAA) surface preconditioning on bonding strength were also studied. The results show that the ionomers bind to HA significantly more strongly than to FA in all cases. The resin-modified material showed a significantly higher shear strength to apatites than the conventional one. Acid etching increased the shear strength significantly for the conventional glass ionomer to both HA and FA, and 25% PAA preconditioning increased the shear strength significantly for the resin-modified glass ionomer to both HA and FA. It was concluded that glass ionomers seemed to bind to apatite chemically, and the bonding strength was influenced by the cohesive strength of the ionomers and the surface roughness of the apatites. The dense synthetic apatites seemed to be good test materials for bonding evaluations of glass ionomers to mineral tissue.

Acid Etching, Dental↗

PubMed1975

Calcification of rachitic rat cartilage in vitro by extracellular matrix vesicles.

Growth plate cartilage from rachitic rats was studied to assess the role in calcification of extracellular matrix vesicles, which are thought to participate in the initial stage of mineralization of connective tissue. The concentration of matrix vesicles and their distribution within the longitudinal septa was found to be normal in rats made rachitic by feeding by a diet low in vitamin D and phosphate for 3 weeks after weaning. Rachitic cartilage matrix did not contain circumvesicular clusters of apatite as does normal cartilage; however, occasional vesicles did enclose one or a few apatite needles. When slices of rachitic cartilage were incubated at 37 C in a metastable calcium phosphate solution ([Ca++] times [PO SEE ARTICLE] equals 3.5 mM identical to 2), apatite formation was initiated in association with matrix vesicles. Under these conditions, mineralization was prominent in the upper hypertrophic cartilage, where matrix vesicles became encrusted with apatite after only 2 to 3 hours of incubation. Vesicular apatite accumulation was inhibited by preheating the cartilage to 60 C for 30 minutes. Measurements of 45Ca uptake by rachitic cartilage slices from metastable calcium phosphates solution also indicated inhibition of calcification by heat. Light microscopic autoradiographs showed 45Ca localization primarily in the matrix of longitudinal septa and substantiated the inhibition site of mineralization in healing rachitic cartilage. The presence of apatite within rachitic vesicles prior to heating and the inhibition of vesicle calcification by heat suggests an active, enzymatically and mediated mechanism of vesicular calcification.

Animals↗

PubMedDate not supplied

[Structure of primary prostatic endogenous calculi].

A crystallographic analysis ("fine plate") is carried out on a total of 62 primary or endogenous prostate stones and the particular features of their structures are described. We observed that they present a compact nucleus consisting of just apatite or whitlockite or of mixtures of the first with other minority components, with apatite (basically carbo-apatite) being the essential component in 98.38% of the stones studied. The periphery present concentric layers, some of which are lobe-shaped, intercalated in cases of mixed periphery and in which there is a qualitative and quantitative predominance of apatite, which may be the only component of the same. The most frequent observation is the association of layers of apatite intercalated with whitlockite to which fine, oxalic or uric layers may sometimes be added. There is sometimes no apatite in the periphery in which case this is made up of layers of whitlockite either interspersed or not with other oxalic or uric ones.

Aged↗

PubMed1984

Formation and transformation of octacalcium phosphate, OCP: a preliminary report.

Octacalcium phosphate, Ca8H2(PO4)6 X 5H2O (OCP), occurs in pathological calcifications frequently as one of the crystalline components of human dental calculi. OCP has also been presumed a necessary precursor of biological apatites in both normal (enamel, dentine, cementum, bones) and pathological (e.g., phosphatic renal stones) calcifications. This study investigated the optimum conditions for the direct in vitro formation of OCP in solutions and in gel systems and the factors affecting its formation and transformation or hydrolysis to apatite. It was observed in both solution and gel systems that the formation of OCP was dependent on definite conditions of pH and temperature (the higher the temperature the lower the pH at which OCP forms, and vice versa), and on the presence of other ions. The presence of pyrophosphate inhibited OCP formation favoring instead the formation of amorphous calcium phosphate while the presence of citrate or carbonate favored the formation of "apatitic" calcium phosphate at the expense of OCP. The presence of oxalate ions caused the formation of mixed OCP/calcium oxalate phases. Hydrolysis of OCP to apatite was suppressed in the presence of magnesium or pyrophosphate, and promoted in the presence of carbonate or fluoride ions. In the presence of oxalate ions, partial hydrolysis of OCP to calcium oxalate and not to apatite was observed. Results from this study give insights on the factors (e.g., pH, temperature, presence of ions besides calcium and phosphate) which influence the formation of OCP and its transformation to apatite and/or calcium oxalate. Ions which demonstrated significant effect on the formation and/or transformation of OCP were magnesium, pyrophosphate, carbonate, citrate, fluoride and oxalate.

Apatites↗

PubMed1998

Interaction of amelogenin with hydroxyapatite crystals: an adherence effect through amelogenin molecular self-association.

At the secretory stage of tooth enamel formation the majority of the organic matrix is composed of amelogenin proteins that are believed to provide the scaffolding for the initial carbonated hydroxyapatite crystals to grow. The primary objective of this study was to investigate the interaction between amelogenins and growing apatite crystals. Two in vitro strategies were used: first, we examined the influence of amelogenins as compared to two other macromolecules, on the kinetics of seeded growth of apatite crystals; second, using transmission electron micrographs of the crystal powders, based on a particle size distribution study, we evaluated the effect of the macromolecules on the aggregation of growing apatite crystals. Two recombinant amelogenins (rM179, rM166), the synthetic leucine-rich amelogenin polypeptide (LRAP), poly(L-proline), and phosvitin were used. It was shown that the rM179 amelogenin had some inhibitory effect on the kinetics of calcium hydroxyapatite seeded growth. The inhibitory effect, however, was not as destructive as that of other macromolecules tested. The degree of inhibition of the macromolecules was in the order of phosvitin > LRAP > poly(L-proline) > rM179 > rM166. Analysis of particle size distribution of apatite crystal aggregates indicated that the full-length amelogenin protein (rM179) caused aggregation of the growing apatite crystals more effectively than other macromolecules. We propose that during the formation of hydroxyapatite crystal clusters, the growing apatite crystals adhere to each other through the molecular self-association of interacting amelogenin molecules. The biological implications of this adherence effect with respect to enamel biomineralization are discussed.

Amelogenin↗

PubMed1996

Osteogenic differentiation of cultured marrow stromal stem cells on the surface of bioactive glass ceramics.

To investigate the significance of apatite-wollastonite-containing glass ceramic (AW ceramic) surfaces and the biological apatite layer formed on these surfaces, rat marrow cell culture, which shows osteogenic differentiation, was carried out on four different culture substrata (control culture dish, two AW ceramics, each having a different surface roughness, and a ceramic on which an apatite layer was formed. A culture period of 2 weeks in the presence of beta-glycerophosphate, ascorbic acid, and dexamethasone resulted in abundant mineralized nodule formations that were positive for alkaline phosphatase (ALP) stain on all substrata. The stain on the apatite-formed AW ceramic was the most intense, the enzyme activity being about twice that of the control culture dish, which had the lowest stain and activity of the four substrata. Northern blot analysis of bone Gla protein (BGP) showed the same tendency, that is, the amount of BGP mRNA from cultured cells on the apatite-formed AW ceramics was the highest and the mRNA on the control dish was the lowest. These data indicate that the glass ceramic surface promotes osteoblastic differentiation and that the promotion can be further enhanced by the formation of a biological apatite layer on the ceramic surface.

Alkaline Phosphatase↗

PubMed1998

Calcium phosphate induction by sol-gel-derived titania coatings on titanium substrates in vitro.

Titanium and its alloys are used widely in the manufacture of orthopedic and dental implants. Sol-gel-prepared titania is able to stimulate bone-like apatite formation in in vitro and in vivo cultures. These materials can be used, for example, as coatings on dental and orthopedic implants. However, the processes that lead to apatite formation are not fully understood. In this study different kinds of titania coatings on commercially pure titanium (c.p. Ti) were tested for apatite-forming ability. The rate of apatite formation is considered to be descriptive of a material's bioactive (bone-bonding) potential. Apatite-forming tests were done in simulated body fluid (SBF). Apatite-forming ability was highest with the addition of valeric acid to sol (600 degrees C) or with sintering sol-gel coatings at 450 degrees-550 degrees C. At that temperature range calcium phosphate forms on the coatings in 1 week. Calcium phosphate forming is observed in 1 day on standard coatings sintered at 500 degrees C.

Biocompatible Materials↗

PubMed2004

A low-temperature biomimetic calcium phosphate surface enhances early implant fixation in a rat model.

The present study demonstrates increased early mechanical fixation of titanium implants coated with a new biomimetic apatite surface in a rat model. Male Sprague-Dawley rats received unilateral femoral medullary implants for periods of 1-4 weeks. The strength of fixation of the implant to the host bone increased more rapidly in the group receiving apatite-treated implants compared with the control group as evidenced by the apatite group's 21-fold greater fixation strength at 1 week (p = 0.009), 4-fold greater fixation strength at 2 weeks (p = 0.041), and 2-fold greater fixation strength at 4 weeks (p = 0.093) compared with the control. Fixation strength was correlated with bone-implant contact as determined from micro computed tomography assessment of the specimens (r2 = 0.338, p = 0.011 in the control group and r2 = 0.543, p < 0.001 in the apatite group). Furthermore, for a given amount of bone-implant contact, the fixation strength was higher in the apatite group than in the control group (p = 0.011), suggesting that the bone formed a stronger bond to the apatite coating than to the titanium. This difference in bonding strength accounted for the difference in mechanical behavior.

Animals↗

PubMed2006

Novel silicon-doped hydroxyapatite (Si-HA) for biomedical coatings: an in vitro study using acellular simulated body fluid.

Magnetron co-sputtering was used to produce silicon-doped hydroxyapatite (Si-HA) as coatings intended for potential applications such as orthopedic and dental implants. It was found that the crystallinity of the as-sputtered coatings increased after annealing, resulting in a nanocrystalline apatite structure. Subsequently, the bioactivity of the coatings was evaluated in an acellular simulated body fluid (SBF). Physicochemical evaluation demonstrated that a carbonate-containing apatite layer, which is essential for bonding at the bone/implant interface, was formed on the coating surfaces after immersion in SBF between 4 and 7 days. The annealed coatings exhibited enhanced bioactivity and chemical stability under physiological conditions, as compared with the as-sputtered coatings. It is proposed that the rate at which the carbonate-containing apatite layer forms is dependent on the scale factor of the structure. A nanocrystalline structure can provide a higher number of nucleation sites for the formation of apatite crystallites, leading to a more rapid precipitation of carbonate-containing apatite layer. This work shows that Si-HA coatings offer considerable potential for applications in hard tissue replacement, owing to their ability to form a carbonate-containing apatite layer rapidly.

Body Fluids↗

PubMed2006

Surface chemistry and biological responses to synthetic octacalcium phosphate.

Octacalcium phosphate (OCP) has been suggested as a precursor of biological apatite in bone, dentin, and cementum because its existence explains the nonstoichiometry of apatite crystals in their compositions. Synthetic inorganic calcium phosphate compounds have been used clinically to fill bone defects, and sintered hydroxyapatite (HA) and beta-tricalcium phosphate (beta-TCP), bone substitute materials, are known to be osteoconductive, with beta-TCP also being bioresorbable. Nonsintered synthetic OCP has been shown to enhance bone regeneration accompanied by conversion into hydrolyzed apatitic products in situ and biodegradation. The surfaces of the OCP implant and the converted apatite seem to be continuously exposed to biological constituents, such as extracellular matrices, inorganic biominerals, and cellular components. This article reviews the surface reaction of OCP implants and the biological responses, such as experimentally stimulated bone formation on synthetic OCP, the mechanism of OCP hydrolysis into apatite, and the adsorption of biomolecules onto OCP and the converted apatite, of particular interest in reactive bone induction with synthetic OCP implants.

Adsorption↗

PubMed1993

Induction and morphology of hydroxyapatite, precipitated from metastable simulated body fluids on sol-gel prepared silica.

Hydroxyapatite crystallization is induced at 37 degrees C by sol-gel prepared silica from metastable calcium phosphate solutions. The morphology of the apatite forming on the silica surface depends on the nature of the solutions. For example, apatite grew in a flake-like form at pH 7.4. The morphology changed to plate-like when the pH was adjusted to pH 7.2. At this lower pH, the apatite plate even exhibited a hexagonal feature, reflecting the unique hexagonal structure of hydroxyapatite. An increase in either Mg or P ion concentration of the fluid can cause apatite to grow in a rod-like shape while addition of F ions to the fluid leads to a perfect needle pattern. The flake geometry of apatite was not altered by increasing Ca concentration from 2.5 to 3.8 mM in the solution. From this we conclude that sol-gel prepared silica is an efficient apatite inducer and the morphology of the hydroxyapatite deposit is determined by factors of the fluid such as pH, Ca/P molar ratio, Mg and F concentrations.

Body Fluids↗

PubMed2000

Formation of a bioactive graded surface structure on Ti-15Mo-5Zr-3Al alloy by chemical treatment.

Simple NaOH and heat treatments provided a Ti-15Mo-5Zr-3Al alloy with a bioactive graded surface structure of an amorphous sodium titanate, where the sodium titanate on the top surface gradually changed into the alloy substrate through titanium oxide. The sodium titanate was free of alloying species of Mo, Zr and Al, since almost all of them were released from the surface of alloy during the first NaOH treatment. The sodium titanate transformed into a hydrated titania via Na+ ion release to induce a bone-like apatite formation on the alloy substrate in a simulated body fluid (SBF). The alloying species neither were released into the SBF nor affected the apatite formation. In the process of apatite formation, the graded surface structure developed into one where the apatite on the top surface gradually changed into the alloy composition through hydrated titania and titanium oxide. It is expected that this graded structure will lead to a strong interfacial bonding strength between the apatite layer and the alloy substrate, thereby providing a tight integration of the alloy with living bone through the apatite layer.

Alloys↗

PubMedDate not supplied

Development of bioactive PMMA-based cement by modification with alkoxysilane and calcium salt.

Poly (methyl methacylate) (PMMA) bone cement is one of the popular bone-repairing materials for fixation of artificial hip joints. Significant problems on the PMMA bone cement are caused by loosening at the interface between bone and the cement, since the cement does not show bone-bonding, i.e. bioactivity. Development of PMMA bone cement capable of bone-bonding has been therefore long desired. The prerequisite for an artificial material to show bone-bonding is the formation of a biologically active bone-like apatite layer on its surface when implanted in the body. The same type of apatite formation can be observed on bioactive materials even in a simulated body fluid (Kokubo solution) with ion concentrations nearly equal to those of human blood plasma. Fundamental researches for bioactive glasses and glass-ceramics revealed that the apatite deposition is initiated by release of Ca2+ ions from the material into the body fluid, and by catalytic effect of Si-OH groups formed on the surface of the material. These findings lead an idea that novel bioactive cement can be designed by incorporation of Si-OH groups and Ca2+ ion into PMMA bone cement. In the present study, PMMA bone cement is modified with 20 mass % of various kinds of alkoxysilanes and calcium salts, and its apatite-forming ability was evaluated in Kokubo solution. The apatite formation was observed on the surface of the modified cements containing 20 mass % of CaCl2, irrespective of the kind of the examined alkoxysilane. On the other hand, the apatite formation was observed on the cement containing CaCl2, Ca(CH3COO)2 or Ca(OH)2, but not on the cement containing CaCO3 or beta-Ca3(PO4)2, even when the cement contains 3-methacryloxypropyltrimethoxysilane (MPS). The results indicate that modification with alkoxysilane and calcium salts showing high water-solubility is effective for providing PMMA bone cement with bioactivity.

Journal Article↗

PubMed2002

Cell adhesion and proliferation on biomimetic calcium-phosphate coatings produced by a sodium silicate gel methodology.

The present study describes a methodology to produce bioactive coatings on the surface of starch based biodegradable polymers or other polymeric biomaterials. As an alternative to the more typical bioactive glass percursors, a sodium silicate gel is being employed as a nucleating agent, for inducing the formation of a calcium-phosphate (Ca-P) layer. The method has the advantage of being able to coat efficiently both compact materials and porous 3D architectures aimed at being used on tissue replacement applications and as bone tissue engineering scaffolds. This treatment is also very effective in reducing the incubation periods, being possible to observe the formation of an apatite-like layer, only after 6 h of immersion in a simulated body fluid (SBF). The influence of the SBF concentration on the formation of the apatite coating was also studied. The apatite coatings formed under different conditions were analyzed and compared in terms of morphology, chemical composition and structure. After the first days of SBF immersion, the apatite-like films exhibit the typical cauliflower like morphology. With increasing immersion times, these films exhibited a partially amorphous nature and the Ca/P ratios became very closer to the value attributed to hydroxyapatite (1.67). The obtained results are very promising for pre-calcifying bone tissue engineering scaffolds. Therefore, in order to study cell behavior and response to these apatite coatings, adhesion, morphology, and proliferation of a human osteoblast cell line (SaOS-2) was also analyzed after being cultured in the coatings formed after 15 days of immersion in SBF. Results indicate a good correlation between crystallinity of the apatite like coatings formed in these conditions and respective cell spreading and morphology. In general, higher cell proliferation was observed for higher crystalline Ca-P coatings.

Journal Article↗

PubMed1996

Preparation of bioactive Ti and its alloys via simple chemical surface treatment.

A simple chemical method was established for inducing bioactivity of Ti and its alloys. When pure Ti, Ti-6A1-4V, Ti-6A1-2Nb-Ta, and Ti-15Mo-5Zr-3A1 substrates were treated with 10M NaOH aqueous solution and subsequently heat-treated at 600 degrees C, a thin sodium titanate layer was formed on their surfaces. Thus, treated substrates formed a dense and uniform bonelike apatite layer on their surfaces in simulated body fluid (SBF) with ion concentrations nearly equal to those of human blood plasma. This indicates that the alkali- and heat-treated metals bond to living bone through the bonelike apatite layer formed on their surfaces in the body. The apatite formation on the surfaces of Ti and its alloys was assumed to be induced by a hydrated titania which was formed by an ion exchange of the alkali ion in the alkali titanate layer and the hydronium ion in SBF. The resultant surface structure changed gradually from the outermost apatite layer to the inner Ti and its alloys through a hydrated titania and titanium oxide layers. This provides not only the strong bonding of the apatite layer to the substrates but also a uniform gradient of stress transfer from bone to the implants. The present chemical surface modification is therefore expected to allow the use the bioactive Ti and its alloys as artificial bones even under load-bearing conditions.

Alkalies↗