Biocompatibility of Ceramic Materials in Ca2P2O7–Ca(PO3)2 System Obtained via Heat Treatment of Cement-Salt Stone

Biocompatibility of ceramic materials in Ca2P2O7-Ca(PO3)2 system was investigated using different methods, including in vitro and in vivo tests. Ceramic materials in the Ca2P2O7-Ca(PO3)2 system were obtained by annealing cement-salt stone based on powder mixtures of calcium citrate tet-rahydrate Ca3(C6H5O7)2·4H2O and monocalcium phosphate monohydrate (MCPM) Ca(H2PO4)2·H2O. The phase composition of cement-salt stone included brushite, monetite as a result of chemical reaction of starting components after adding of water. The presence of citric acid as by-product of chemical reaction, leads to increase the setting time of the cement-salt stone. Highly concentrated aqueous suspensions based on calcium citrate and MCPM powders providing content of calcium polyphosphate Ca(PO3)2 up to 20 wt % in ceramics were used for designing bioresorbable materials. The presence of an excess of monocalcium phosphate monohydrate makes it possible to reduce the annealing temperature of ceramics, which is associated with the formation of a lower melting phase of Ca(PO3)2. In vivo tests shown that obtained ceramic materials can be recommended for regenerative treatments for bone defects

Ceramic Materials in Na2O-CaO-P2O5 System, Obtained via Heat Treatment of Cement-Salt Stone Based on Powder Mixture of Ca3(C6H5O7)2∙4H2O, Ca(H2PO4)2∙H2O and NaH2PO4

Ceramic materials in Na2O-CaO-P2O5 system were obtained by firing cement-salt stone made from pastes based on powder mixtures including calcium citrate tetrahydrate Ca3(C6H5O7)2∙4H2O, monocalcium phosphate monohydrate (MCPM) Ca(H2PO4)2∙H2O and/or sodium dihydrogen phosphate NaH2PO4. The phase composition of the obtained samples of cement-salt stone after adding water, hardening and drying included brushite CaHPO4∙2H2O, monetite CaHPO4 and also unreacted Ca3(C6H5O7)2∙4H2O, Ca(H2PO4)2∙H2O and/or NaH2PO4. The phase composition of ceramics in Na2O-CaO-P2O5 system obtained by firing cement-salt stone was formed due to thermal conversion of hydrated salt and heterophase reactions between components presented in samples during firing. The phase composition of ceramic samples based on powder mixture of Ca3(C6H5O7)2∙4H2O and Ca(H2PO4)2∙H2O after firing at 900 °C included β-calcium pyrophosphate (CPP) β-Ca2P2O7. The phase composition of ceramic samples based on powder mixture of Ca3(C6H5O7)2∙4H2O, and NaH2PO4 after firing at 900 °C included β-sodium rhenanite β-CaNaPO4. The phase composition of ceramic samples based on powder mixture of Ca3(C6H5O7)2∙4H2O, Ca(H2PO4)2∙H2O and NaH2PO4 after firing at 900 °C included β-Ca2P2O7, β-CaNaPO4, double calcium-sodium pyrophosphate Na2CaP2O7, and Na-substituted tricalcium phosphate Сa10Na(PO4)7. Obtained ceramic materials in Na2O-CaO-P2O5 system including biocompatible and biodegradable phases could be important for treatments of bone tissue defects by means of approaches of regenerative medicine

Ceramics Based on Sodium Rhenanite CaNaPO₄, Obtained via Firing of Composite Cement-Salt Stone

Ceramics based on rhenanite CaNaPO4 with density of 0.94 g/cm3 and compressive strength of 10.3 MPa was obtained via firing at 900 °C of composite cement-salt stone prepared from a hardening powder mixture of calcium citrate tetrahydrate Ca3(C6H5O7)2∙4H2O and sodium dihydrogen phosphate NaH2PO4. The phase composition of the obtained samples of cement–salt stone was represented by monetite CaHPO4, unreacted sodium dihydrogen phosphate and calcium citrate tetrahydrate. According to the XRD data, the phase composition of the ceramic samples after annealing in the temperature range of 500–700 °C was mainly represented by the β-CaNaPO4 phase. It was found that after an annealing at temperature of 900 °C, the phase composition of ceramics was presented with the only phase of β-CaNaPO4. It was demonstrated that an increase in the annealing temperature led to an increase in the grain size from 1 μm after annealing at 500 °C to 5 μm after annealing at 900 °C. Obtained ceramic material based on CaNaPO4 could be important for regenerative treatments of bone tissue defects

Biocompatibility of Ceramic Materials in Ca₂P₂O_7–Ca(PO₃)₂ System Obtained via Heat Treatment of Cement-Salt Stone

Biocompatibility of ceramic materials in Ca2P2O7-Ca(PO3)2 system was investigated using different methods, including in vitro and in vivo tests. Ceramic materials in the Ca2P2O7-Ca(PO3)2 system were obtained by annealing cement-salt stone based on powder mixtures of calcium citrate tet-rahydrate Ca3(C6H5O7)2·4H2O and monocalcium phosphate monohydrate (MCPM) Ca(H2PO4)2·H2O. The phase composition of cement-salt stone included brushite, monetite as a result of chemical reaction of starting components after adding of water. The presence of citric acid as by-product of chemical reaction, leads to increase the setting time of the cement-salt stone. Highly concentrated aqueous suspensions based on calcium citrate and MCPM powders providing content of calcium polyphosphate Ca(PO3)2 up to 20 wt % in ceramics were used for designing bioresorbable materials. The presence of an excess of monocalcium phosphate monohydrate makes it possible to reduce the annealing temperature of ceramics, which is associated with the formation of a lower melting phase of Ca(PO3)2. In vivo tests shown that obtained ceramic materials can be recommended for regenerative treatments for bone defects

Bioceramics Based on β-Calcium Pyrophosphate

Ceramic samples based on β-calcium pyrophosphate β-Ca2P2O7 were prepared from powders of γ-calcium pyrophosphate γ-Ca2P2O7 with preset molar ratios Ca/P = 1, 0.975 and 0.95 using firing at 900, 1000, and 1100 °C. Calcium lactate pentahydrate Ca(C3H5O3)2⋅5H2O and monocalcium phosphate monohydrate Ca(H2PO4)2⋅H2O were treated in an aqua medium in mechanical activation conditions to prepare powder mixtures with preset molar ratios Ca/P containing calcium hydrophosphates with Ca/P = 1 (precursors of calcium pyrophosphate Ca2P2O7). These powder mixtures containing calcium hydrophosphates with Ca/P = 1 and non-reacted starting salts were heat-treated at 600 °C after drying and disaggregation in acetone. Phase composition of all powder mixtures after heat treatment at 600 °C was presented by γ-calcium pyrophosphate γ-Ca2P2O7 according to the XRD data. The addition of more excess of monocalcium phosphate monohydrate Ca(H2PO4)2·H2O (with appropriate molar ratio of Ca/P = 1) to the mixture of starting components resulted in lower dimensions of γ-calcium pyrophosphate (γ-Ca2P2O7) individual particles. The grain size of ceramics increased both with the growth in firing temperature and with decreasing molar ratio Ca/P of powder mixtures. Calcium polyphosphate (t melt = 984 °C), formed from monocalcium phosphate monohydrate Ca(H2PO4)2⋅H2O, acted similar to a liquid phase sintering additive. It was confirmed by tests in vitro that prepared ceramic materials with preset molar ratios Ca/P = 1, 0.975, and 0.95 and phase composition presented by β-calcium pyrophosphate β-Ca2P2O7 were biocompatible and could maintain bone cells proliferation

Low-Temperature Magnesium Calcium Phosphate Ceramics with Adjustable Resorption Rate

Low-temperature ceramics based on magnesium calcium phosphate cement are a promising resorbable material for bone tissue restoration with the possibility of functionalization. The replacement of the magnesium Mg2+ ion with a calcium Ca2+ ion at the stage of preparation of the precursor leads to the production of multiphase ceramics containing phases of brushite, monetite, and newberyite, with different dissolution rates. Multiphase ceramics leads to volumetric resorption with preservation of their geometric shape, which was confirmed by the results of an evaluation of the output of magnesium Mg2+ and calcium Ca2+ ions into the contact solution of the ceramics and the X-ray density of ceramic samples during subcutaneous implantation. The combined introduction of sodium pyrophosphate decahydrate and citric acid monohydrate as setting inhibitors neutralizes their insignificant negative effect on the physico-chemical properties of ceramics (strength, pH, porosity), determining the optimal composition. In vivo experiments with setting inhibitors in the composition of ceramics showed a different biological response, affecting the rate of resorption on par with magnesium ions. Preliminary data on biocompatibility and solubility determined magnesium-calcium phosphate ceramics containing additives that regulate setting to be a potential material for bone tissue restoration and a vector for further research, including in orthotopic implantation models

Inorganic Powders Prepared from Fish Scales

A mixture of abramis brama (freshwater bream), carassius carassius (crucian carp), and sander lucioperca (pike perch) scales was used for the preparation of fish scale powder containing constituents of organic and inorganic nature. The mixture of the mentioned fish scales was washed, dried, and ground for the preparation of fish scale powder. Vibration sieving was used to prepare fish scale powder enriched with inorganic components. According to thermal analysis data, this fish scale powder enriched with inorganic components included about 36.5 wt.% components removed when heating, primarily those of organic nature, and 63.5 wt.% mineral components. Inorganic powders consisting of hydroxyapatite and magnesium whitlockite were obtained via heat treatment of this fish scale powder at 800–1000 °C. Particles of these inorganic powders consisted of sintered grains with dimensions less than 100 nm after heat treatment at 800 °C, less than 200 nm after heat treatment at 900 °C, and 100–1000 nm after heat treatment at 1000 °C. Fish scale powder enriched with inorganic components as well as heat-treated inorganic powders consisting of hydroxyapatite and magnesium whitlockite can be recommended for the production of different materials, such as ceramics or composites

Inorganic Powders Prepared from Fish Scales

A mixture of abramis brama (freshwater bream), carassius carassius (crucian carp), and sander lucioperca (pike perch) scales was used for the preparation of fish scale powder containing constituents of organic and inorganic nature. The mixture of the mentioned fish scales was washed, dried, and ground for the preparation of fish scale powder. Vibration sieving was used to prepare fish scale powder enriched with inorganic components. According to thermal analysis data, this fish scale powder enriched with inorganic components included about 36.5 wt.% components removed when heating, primarily those of organic nature, and 63.5 wt.% mineral components. Inorganic powders consisting of hydroxyapatite and magnesium whitlockite were obtained via heat treatment of this fish scale powder at 800–1000 °C. Particles of these inorganic powders consisted of sintered grains with dimensions less than 100 nm after heat treatment at 800 °C, less than 200 nm after heat treatment at 900 °C, and 100–1000 nm after heat treatment at 1000 °C. Fish scale powder enriched with inorganic components as well as heat-treated inorganic powders consisting of hydroxyapatite and magnesium whitlockite can be recommended for the production of different materials, such as ceramics or composites

Chemically Bound Resorbable Ceramics as an Antibiotic Delivery System in the Treatment of Purulent–Septic Inflammation of Bone Tissue

Local drug delivery systems are an effective approach in the treatment of purulent–septic inflammation of bone tissue. Chemically bonded multiphase ceramics based on calcium-deficient carbonate-substituted hydroxyapatite combine resorbability, osteoconductivity, and the possibility of volumetric incorporation of antibiotics. Macroporosity is regulated by the concentration of polyethylene glycol granules introduced into the initial powder composition, followed by their extraction. The selected conditions for the consolidation of the ceramic matrix and the extraction of PEG granules retain the activity of vancomycin, which is confirmed by the results of microbiological studies. The concentration of vancomycin and the porosity affect the local concentration and release of the antibiotic. The incorporation method provides a prolonged release of the antibiotic for up to 31 days. In vivo experiments with bone implantation have shown that chemically bound macroporous ceramics with incorporated vancomycin are a therapeutically effective carrier of the substance during the healing of bone defects in conditions of surrounding purulent–septic inflammation, and can be considered as a carrier for local antibacterial therapy, at the site of implantation