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Bone defects resulting from trauma, diseases, or surgical procedures pose significant challenges in the field of oral and maxillofacial surgery. The development of effective bone substitute materials that promote bone healing and regeneration is crucial for successful clinical outcomes. Calcium phosphate cements (CPCs) have emerged as promising candidates for bone replacement due to their biocompatibility, bioactivity, and ability to integrate with host tissues. However, there is a continuous demand for further improvements in the mechanical properties, biodegradability, and bioactivity of these materials. Dual setting of cements is one way to improve the performance of CPCs. Therefore, silicate matrices can be incorporated in these cements. Silicate-based materials have shown great potential in various biomedical applications, including tissue engineering and drug delivery systems. In the context of bone regeneration, silicate matrices offer unique advantages such as improved mechanical stability, controlled release of bioactive ions, and enhanced cellular responses. Comprehensive assessments of both the material properties and biological responses of our samples were conducted. Cytocompatibility was assessed through in vitro testing using osteoblastic (MG-63) and osteoclastic (RAW 264.7) cell lines. Cell activity on the surfaces was quantified, and scanning electron microscopy (SEM) was employed to capture images of the RAW cells. In our study, incorporation of tetraethyl orthosilicate (TEOS) in dual-curing cements significantly enhanced physical properties, attributed to increased crosslinking density and reduced pore size. Higher alkoxysilyl group concentration improved biocompatibility by facilitating greater crosslinking. Additionally, our findings suggest citrate's potential as an alternative retarder due to its positive interaction with the silicate matrix, offering insights for future dental material research. This paper aims to provide an overview of the importance of silicate matrices as modifiers for calcium phosphate cements, focusing on their impact on the mechanical properties, setting behaviour, and biocompatibility of the resulting composites. [ABSTRACT FROM AUTHOR]

The influence of two nanostructured osteoplastic materials with different compositions: i) alginate (Alg) matrix, loaded with Zn2+ ions and nanostructured hydroxyapatite (HA) - S1/HA-Zn, and ii) chitosan (CS) matrix loaded with brushite nanoparticles (NPs, dicalcium phosphate dihydrate, DCPD) - S2/DCPD on the healing of an experimental femoral diaphysis defect was investigated. The structure of cellular elements and the lacunar tubular system of the regenerated bone tissue were studied by electron microscopy. Osteogenic cells on the surface and inside S1/HA-Zn formed bone tissue. On the 30th day, the latter had a reticulofibrous and later lamellar structure. On the 30th day, the S2/DCPD biomaterial was integrated mainly into connective tissue and, starting from the 90th day, into the bone tissue, which was formed only on its outer surface. Thus, it has been proven that both biomaterials contribute to the healing of bone wounds. The regenerative potential of the new bone tissue formation of S1/HA-Zn prevails over that of S2/DCPD.

The wastewater treatment industry could benefit from new technologies for the removal and recovery of phosphorus (P). The CalPrex precipitation reactor has the potential to recover P in a readily land-applicable form by treating organic acid digestate with calcium hydroxide to produce brushite. Using data from a pilot-scale reactor at the local Nine Springs Wastewater Treatment Plant in Madison, WI, we modified the plant's BioWin configuration using BioWin 6.2 to model the CalPrex technology and estimate performance under a variety of conditions. We produced dose/response curves for a range of possible lime dosages to estimate the impact of reagent dosage on the quantity and composition of precipitate produced by the CalPrex reactor and characterize the effects on downstream anaerobic digester performance. CalPrex was found to capture 46% of the plant's influent P, reducing nuisance struvite precipitates by 57% and biosolid sludge production by 14%. The CalPrex module was also tested in two predesigned plant configurations in the BioWin cabinet with the intention of testing applicability to other configurations and searching for the impacts of CalPrex on treatment train performance. This is the first work simulating a full-scale implementation of CalPrex and the first to model interactions of CalPrex with other treatment processes. [ABSTRACT FROM AUTHOR]

Composite polylactide materials based on hydrated calcium phosphates (amorphized hydroxyapatite and brushite) promising for 3D printing of osteoplastic biomaterials are obtained by an extrusion method. The formation of coatings containing amorphized hydroxyapatite promotes 1.5- to 3.5-fold strengthening of three-dimensional models based on such composite materials and leads to hydrophilization of their surface. [ABSTRACT FROM AUTHOR]

In recent years, significant developments have taken place in scientific fields such as tissue and materials engineering, which allow for the development of new, intelligent biomaterials. An example of such biomaterials is drug delivery systems that release the active substance directly at the site where the therapeutic effect is required. In this research, polymeric materials and ceramic–polymer composites were developed as carriers for the antibiotic clindamycin. The preparation and characterization of biomaterials based on hyaluronic acid, collagen, and nano brushite obtained using the photocrosslinking technique under UV (ultraviolet) light are described. Physical and chemical analyses of the materials obtained were carried out using Fourier transform infrared spectroscopy (FT-IR) and optical microscopy. The sorption capacities were determined and subjected to in vitro incubation in simulated biological environments such as Ringer's solution, simulated body fluid (SBF), phosphate-buffered saline (PBS), and distilled water. The antibiotic release rate was also measured. The study confirmed higher swelling capacity for materials with no addition of a ceramic phase, thus it can be concluded that brushite inhibits the penetration of the liquid medium into the interior of the samples, leading to faster absorption of the liquid medium. In addition, incubation tests confirmed preliminary biocompatibility. No drastic changes in pH values were observed, which suggests that the materials are stable under these conditions. The release rate of the antibiotic from the biomaterial into the incubation medium was determined using high-pressure liquid chromatography (HPLC). The concentration of the antibiotic in the incubation fluid increased steadily following a 14-day incubation in PBS, indicating continuous antibiotic release. Based on the results, it can be concluded that the developed polymeric material demonstrates potential for use as a carrier for the active substance. [ABSTRACT FROM AUTHOR]

Calcium phosphate coatings containing brushite, calcite, and apatite were obtained by electrochemical deposition on titanium plates at room temperature, pH 5, constant current density 30 mA/cm2, from CaCO3/Ca(H2PO4)2 suspension electrolyte. A layer of amorphous apatite was deposited by the biomimetic method, by keeping the coatings in a concentrated modeling solution of Simulated Body Fluid. As a result of heat treatment at 800°C, apatite crystallized into hydroxyapatite, calcite decomposed to calcium oxide, and titanium was covered with a layer of titanium (IV) oxide. Preclinical studies on rats in vivo for 3 months showed increased osseointegration of plates with calcium phosphate coatings compared to uncoated titanium. Titanium implants with calcium phosphate coatings enriched with hydroxyapatite are promising for use in neurosurgery, dentistry, orthopedics due to the absence of inflammatory reactions from the body and increased osseointegration.

Acid, medium, and basic calcium phosphates were obtained by liquid-phase synthesis from aqueous solutions of calcium chloride and ammonium hydrogen phosphate at Ca/P molar ratios of 1,0-1,67 and pH 5-11 in the presence of a polyphenol compound (gallic acid). Using X-ray phase analysis and IR spectroscopy, it has been shown that brushite is formed in a slightly acidic medium (pH 5-6) at a Ca/P molar ratio of 1,0, the unit cell size of which can decrease in the presence of gallic acid. In an alkaline environment (pH 8-11), the polyphenolic compound chelates calcium ions, which leads to the formation of amorphized calcium phosphate, which after heating at 800°C turns into β-tricalcium phosphate and hydroxyapatite. It was found that the presence of gallic acid promotes the formation of basic calcium phosphate at a lower molar ratio (Ca/P 1,5) than for stoichiometric hydroxyapatite (Ca/P 1,67). It has been shown by thermal analysis that the liquid-phase synthesis of calcium phosphates in the presence of gallic acid promotes the transformation of brushite into calcium pyrophosphate, and amorphized calcium phosphates into tricalcium phosphate and hydroxyapatite, upon high-temperature treatment.

Artificial phantoms used in photothermal near-infrared laser lithotripsy research generally fail to mimic both the chemical and the physical properties of human stones. Though high-energy, 1 J pulses are capable of fracturing hard human stones into several large fragments along natural boundaries, similar behavior has not been observed in commonly used gypsum plasters like BegoStone. We developed a new brushite-based plaster formulation composed of ≈90% brushite that undergoes rapid fracture in the manner of human stones under fragmentation pulse regimes. Single-pulse (1 J) ablation crater volumes for phantoms were not significantly different from those of pure brushite stones. Control over crater volumes was demonstrated by varying phosphorous acid concentration in the plaster formulation. Fragmentation of cylindrical brushite phantoms was filmed using a high-speed camera which demonstrated rapid fragmentation in < 100 µs during the bubble expansion phase of a short pulse from a high-powered Ho:YAG laser (Lumenis Pulse 120 H). The rapid nature of observed fracture suggests increasing laser pulse energy by increasing laser pulse duration will not improve fragmentation performance of laser lithotripters. Brushite plaster phantoms are a superior alternative to gypsum plasters for laser lithotripsy research due to their better mimicry of stone composition, controllable single-pulse crater volumes, and fragmentation behavior. [ABSTRACT FROM AUTHOR]

This study aimed to explore the effects of the full-scale replacement (up to 100%) of Ca2+ ions with Ag1+ ions in the structure of brushite (CaHPO4·2H2O). This substitution has potential benefits for producing monophasic and biphasic Ca1−xAgxHPO4·nH2O compounds. To prepare the starting solutions, (NH4)2HPO4, Ca(NO3)2·4H2O, and AgNO3 at different concentrations were used. The results showed that when the Ag/Ca molar ratio was below 0.25, partial substitution of Ca with Ag reduced the size of the unit cell of brushite. As the Ag/Ca molar ratio increased to 4, a compound with both monoclinic CaHPO4·2H2O and cubic nanostructured Ag3PO4 phases formed. There was a nearly linear relationship between the Ag ion ratio in the starting solutions and the wt% precipitation of the Ag3PO4 phase in the resulting compound. Moreover, when the Ag/Ca molar ratio exceeded 4, a single-phase Ag3PO4 compound formed. Hence, adjusting the Ag/Ca ratio in the starting solution allows the production of biomaterials with customized properties. In summary, this study introduces a novel synthesis method for the mono- and biphasic Ca1−xAgxHPO4·nH2O compounds brushite and silver phosphate. The preparation of these phases in a one-pot synthesis with controlled phase composition resulted in the enhancement of existing bone cement formulations by allowing better mixing of the starting ingredients. [ABSTRACT FROM AUTHOR]

Composite cements containing brushite, monetite and newberyite as dominating phases were created and used as drug (vancomycin) carriers. Brushite-monetite-newberyite cement with variable composition was obtained by replacing Ca2+ ions with Mg2+ in the initial cement component. Starting powder mixtures for cement preparation synthesized via solid state reaction consisted of MgxCa(3-х)(PO4)2 (x = 0, 0.75, 1.5, 2.25, 3), monocalcium phosphate monohydrate Ca(H2PO4)2·H2O with and without vancomycin as antibacterial agent. 100 mg of powder of a pharmaceutical substance per 1 g of the dry cement powder was added before cement sample preparation. Mixing liquids used were water solutions containing sodium pyrophosphate hexahydrate Na4P2O7·10H2O and citric acid monohydrate C6H8O7·H2O as set-retarding additives. An increase in the concentration of Mg2+ ions entail an increase in pH during preparation and a decrease in porosity of cement sample. Incorporation of vancomycin at the stage of preparation of the cement mixture does not affect the strength characteristics, porosity and pH of the cement stone. The prolongation of the release of vancomycin depends on the composition and characteristics of the cement stone. The activity of vancomycin against Staphylloccoscus aureus and Escherichia coli the process of hydration of cement and its dissolution was confirmed by appropriate tests in vitro. In vivo studies confirm the biocompatibility, resorbability of cements, and the effectiveness of their use as carriers of vancomycin in the treatment of purulent-septic inflammation.

In vitro studies of stone-related crystals and crystals-cell interactions have been extensively done to investigate cellular, molecular and pathogenic mechanisms leading to renal calculi. Effective preparation of various types of stone-related crystals is thus crucial for such studies. Nevertheless, various protocols for preparing these stone-related crystals were scatteredly reported without comparative analysis of their efficacies and yields. Herein, we systematically compared our protocols (with the suffix “-Si”) for preparing calcium oxalate (CaOx) monohydrate (COM), CaOx dihydrate (COD), magnesium ammonium phosphate (struvite), uric acid (UA), calcium phosphate dihydrate (brushite), hydroxyapatite (HAP), and calcium carbonate (CaCO3) crystals with other protocols published previously. The morphological evaluation revealed that our protocols provided the most homogeneous and most typical monoclinic prismatic, bipyramidal, coffin lid and rectangle shapes of COM, COD, struvite and UA crystals, respectively. There were comparable morphological results for brushite, HAP and CaCO3 crystals generated by different protocols. Our protocols provided the greatest yield for generating brushite crystals but with lower yields for others. Chemical analysis by Fourier transform infrared (FTIR) spectroscopy revealed comparable results among different protocols to generate each crystal type. In summary, all these protocols can be used to generate each crystal type. But our protocols offer the best quality, in terms of homogeneity and typical shape, for generating COM, COD, struvite and UA crystals.

Bone defects resulting from trauma, diseases, or surgical procedures pose significant challenges in the field of oral and maxillofacial surgery. The development of effective bone substitute materials that promote bone healing and regeneration is crucial for successful clinical outcomes. Calcium phosphate cements (CPCs) have emerged as promising candidates for bone replacement due to their biocompatibility, bioactivity, and ability to integrate with host tissues. However, there is a continuous demand for further improvements in the mechanical properties, biodegradability, and bioactivity of these materials. Dual setting of cements is one way to improve the performance of CPCs. Therefore, silicate matrices can be incorporated in these cements. Silicate-based materials have shown great potential in various biomedical applications, including tissue engineering and drug delivery systems. In the context of bone regeneration, silicate matrices offer unique advantages such as improved mechanical stability, controlled release of bioactive ions, and enhanced cellular responses. Comprehensive assessments of both the material properties and biological responses of our samples were conducted. Cytocompatibility was assessed through in vitro testing using osteoblastic (MG-63) and osteoclastic (RAW 264.7) cell lines. Cell activity on the surfaces was quantified, and scanning electron microscopy (SEM) was employed to capture images of the RAW cells. In our study, incorporation of tetraethyl orthosilicate (TEOS) in dual-curing cements significantly enhanced physical properties, attributed to increased crosslinking density and reduced pore size. Higher alkoxysilyl group concentration improved biocompatibility by facilitating greater crosslinking. Additionally, our findings suggest citrate’s potential as an alternative retarder due to its positive interaction with the silicate matrix, offering insights for future dental material research. This paper aims to provide an overview of the importance of silicate matrices as modifiers for calcium phosphate cements, focusing on their impact on the mechanical properties, setting behaviour, and biocompatibility of the resulting composites.

Introduction: Bio-cementation processes [namely, microbial induced carbonate precipitation (MICP) and enzyme induced carbonate precipitation (EICP)] have recently become promising techniques for solidifying loose sands. However, these methods release gaseous ammonia to the atmosphere, which is not desirable for real-scale applications. This study aims to propose an enzyme induced calcium phosphate precipitation (EICPP) method as a sustainable direction for the solidification of sand.Methods: Precipitation of calcium phosphate compound (CPC) was driven through pH-dependent mechanism regulated by enzymatic hydrolysis of urea. The baseline study was designed to consist of a series of precipitation tests and sand column tests, evaluating the influence of various recipes of cementation media (CM) on treatment efficiency. The evaluation program consisted of Unconfined compression tests, precipitation content measurement, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction.Results: The observations showed that the content of urea had an important role in proposed EICPP treatment, which determined the extent of the pH increase. This increase had a great influence on 1) utilization of soluble calcium, 2) precipitation content of calcium phosphate, and 3) the morphology of the precipitates. Results of sand column test suggested that injecting CM that consisted of acid-dissolved bone meal, urea and urease enzyme could result in the deposition of insoluble CPC that enabled the solidification of sand particles.Discussion: The precipitation quantity was found to increase with the increase in urea content; however, the treatment media with high urea content resulted amorphous-like crystals. The plate-like crystals were evidenced in CM with [Ca]/[urea] molar ratio between 1.5–2.0. X-ray Diffraction (XRD) analysis revealed that irrespective of the urea contents, the formed crystals were identified as brushite. Since the final pH of proposed EICPP method could be controllable within acidic-neutral conditions, the emission of ammonia gas would be eliminated.

This study examined the profile of patients and the impact of diet on the risk of brushite stone formation under controlled, standardized conditions. Sixty-five patients with brushite nephrolithiasis were enrolled in the study. Metabolic, dietary, and 24 h urinary parameters were collected under the habitual, self-selected diet of the patients and the balanced mixed, standardized diet. The [13C2]oxalate absorption, ammonium chloride, and calcium loading tests were conducted. All patients had at least one abnormality on the usual diet, with hypercalciuria (84.6%), increased urine pH (61.5%), and hyperphosphaturia (43.1%) being the most common. Absorptive hypercalciuria was present in 32.1% and hyperabsorption of oxalate in 41.2%, while distal renal tubular acidosis (dRTA) was noted in 50% of brushite stone formers. The relative supersaturation of brushite did not differ between patients with and without dRTA. Among all recent brushite-containing calculi, 61.5% were mixed with calcium oxalate and/or carbonate apatite. The relative supersaturation of brushite, apatite, and calcium oxalate decreased significantly under the balanced diet, mainly due to the significant decline in urinary calcium, phosphate, and oxalate excretion. Dietary intervention was shown to be effective and should be an integral part of the treatment of brushite stone disease. Further research on the role of dRTA in brushite stone formation is needed. [ABSTRACT FROM AUTHOR]

This study was carried out to investigate the effect of a complete exchange of Ca2+ with Zn2+ ions on the structure of brushite (CaHPO4·2H2O), which might be advantageous in the production process of CaxZn1−xHPO4·nH2O. To acquire the starting solutions needed for the current study, (NH4)2HPO4, Ca(NO3)2·4H2O, and Zn(NO3)2·6H2O were utilized in several molar concentrations. The findings indicate that Ca is partly substituted by Zn when the Zn/Ca molar ratio is below 0.25 and that Zn doping hinders the crystallization of brushite. A continued increase in the Zn/Ca molar ratio to 1 (at which point the supersaturation of the Zn solution rises) led to a biphasic compound of monoclinic brushite and parascholzite precipitate. Elevating the Zn/Ca molar ratio to 1.5 resulted in a precipitate of a parascholzite-like mineral. Finally, increasing the Zn/Ca molar ratio to 4 and above resulted in the formation of the hopeite mineral. Future biomaterial production with specific and bespoke characteristics can be achieved by adjusting the Zn/Ca ratio in the starting solution. It Rhas been established that the Zn/Ca ratio in the starting solution can be adjusted to obtain minerals with specific compositions. Thus, new synthesis methods for parascholzite and hopeite were introduced for the first time in this manuscript. [ABSTRACT FROM AUTHOR]

Fine powders of brushite CaHPO4·2H2O, ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O), and calcium sulfate dihydrate CaSO4·2H2O—all containing sodium chloride NaCl as a reaction by-product—were synthesized from 0.5 M aqueous solution of calcium chloride CaCl2, sodium hydrophosphate Na2HPO4 and/or sodium sulfate Na2SO4. Powder of ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O) was synthesized by precipitation from aqueous solution of calcium chloride CaCl2 and mixed-anionic solution simultaneously containing the hydrogen phosphate anion HPO42− (Na2HPO4) and sulfate anion SO42− (Na2SO4). Sodium chloride NaCl, presenting in compacts based on synthesized powders of brushite CaHPO4·2H2O, ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O) and calcium sulfate dihydrate CaSO4·2H2O, was responsible for both low-temperature melt formation and the creation of phase composition of ceramics. Heterophase interaction of components led to the resulting phase composition of the ceramic samples during heating, including the formation of chlorapatite Ca5(PO4)3Cl in powders of brushite and ardealite. The phase composition of the ceramics based on the powder of brushite CaHPO4·2H2O containing NaCl as a by-product after firing at 800–1000 °C included β-Ca2P2O7, and Ca5(PO4)3Cl. The phase composition of ceramics based on the powder of ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O) containing NaCl as a by-product after firing at 800 and 900 °C included β-Ca2P2O7, CaSO4, and Ca5(PO4)3Cl; after firing at 1000 °C, it includedCaSO4, Ca5(PO4)3Cl and Ca3(PO4)2/Ca10Na(PO4)7, and after firing at 1100 °C, it included CaSO4 and Ca5(PO4)3Cl. The phase composition of ceramics based on powder of calcium sulfate dihydrate CaSO4·2H2O containing NaCl as a by-product after firing at 800–1100 °C included CaSO4 as the predominant phase. The phase composition of all ceramic samples under investigation consisted of biocompatible crystalline phases with different abilities to biodegrade. For this reason, the created ceramics can be recommended for testing as materials for treatment of bone defects using regenerative medicine methods.

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.

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.

The wastewater treatment industry could benefit from new technologies for the removal and recovery of phosphorus (P). The CalPrex precipitation reactor has the potential to recover P in a readily land-applicable form by treating organic acid digestate with calcium hydroxide to produce brushite. Using data from a pilot-scale reactor at the local Nine Springs Wastewater Treatment Plant in Madison, WI, we modified the plant’s BioWin configuration using BioWin 6.2 to model the CalPrex technology and estimate performance under a variety of conditions. We produced dose/response curves for a range of possible lime dosages to estimate the impact of reagent dosage on the quantity and composition of precipitate produced by the CalPrex reactor and characterize the effects on downstream anaerobic digester performance. CalPrex was found to capture 46% of the plant’s influent P, reducing nuisance struvite precipitates by 57% and biosolid sludge production by 14%. The CalPrex module was also tested in two predesigned plant configurations in the BioWin cabinet with the intention of testing applicability to other configurations and searching for the impacts of CalPrex on treatment train performance. This is the first work simulating a full-scale implementation of CalPrex and the first to model interactions of CalPrex with other treatment processes.

Tri-calcium-phosphate Ca3(PO4)2 is considered a promising material to improve implant and bone tissue linking. Titanium (Ti), a highly porous material, was coated with crystalline brushite using an electrochemical process so that it could be used as an implant material. The aim of this research is to get a faster ingrowth of bone-tissue inside the porous structure. The crystalline coating was characterized by the standard XRD and SEM techniques. Additionally, the phase evolution of Ca3(PO4)2-crystals with different kinds of sterilization techniques was observed. In-vitro tests on the biocompatibility of the coating were done with human mesenchymal stem cells (HMSCs). The HMSCs are the most promising cell type for regenerative medicine and tissue engineering owing to their ability to differentiate into several tissues, such as, bone, cartilage, tendon, and muscle. For the treatment of local bone defects expanded HMSCs could be loaded on Ca3(PO4)2 coated metallic matrices and delivered to the target site. A possible application is brushite-coated porous titanium as a carrier matrix. To determine whether cell functions of HMSCs are influenced by the brushite surface, HMSCs were cultured on brushite-coated and uncoated porous titanium specimens. The viability and proliferation of HMSCs were successfully analyzed. Additionally, the release of cytokines (IL-6, IL-8, IL-11) were quantified as a marker of cell activation. The viable cells could be detected on specimens after 48 h initial seeding. After 8 days cell number on both specimens increased, although the proliferation on brushite-coated titanium was decreased compared to the uncoated surfaces. The release of both, IL-8 and IL-11 increased significantly due to the cultivation of HMSCs on the coated specimens for 8 days.

Interest in calcium phosphate cements as materials for the restoration and treatment of bone tissue defects is still high. Despite commercialization and use in the clinic, the calcium phosphate cements have great potential for development. Existing approaches to the production of calcium phosphate cements as drugs are analyzed. A description of the pathogenesis of the main diseases of bone tissue (trauma, osteomyelitis, osteoporosis and tumor) and effective common treatment strategies are presented in the review. An analysis of the modern understanding of the complex action of the cement matrix and the additives and drugs distributed in it in relation to the successful treatment of bone defects is given. The mechanisms of biological action of functional substances determine the effectiveness of use in certain clinical cases. An important direction of using calcium phosphate cements as a carrier of functional substances is the volumetric incorporation of anti-inflammatory, antitumor, antiresorptive and osteogenic functional substances. The main functionalization requirement for carrier materials is prolonged elution. Various release factors related to the matrix, functional substances and elution conditions are considered in the work. It is shown that cements are a complex system. Changing one of the many initial parameters in a wide range changes the final characteristics of the matrix and, accordingly, the kinetics. The main approaches to the effective functionalization of calcium phosphate cements are considered in the review. [ABSTRACT FROM AUTHOR]

Calcium phosphate-based coatings are widely studied in orthopedics and dentistry for their similarity to the mineral component of bone and their capability to promote osseointegration. Different calcium phosphates have tunable properties that result in different behaviors in vitro, but the majority of studies focus only on hydroxyapatite. Here, different calcium phosphate-based nanostructured coatings are obtained by ionized jet deposition, starting with hydroxyapatite, brushite and beta-tricalcium phosphate targets. The properties of the coatings obtained from different precursors are systematically compared by assessing their composition, morphology, physical and mechanical properties, dissolution, and in vitro behavior. In addition, for the first time, depositions at high temperature are investigated for the further tuning of the coatings mechanical properties and stability. Results show that different phosphates can be deposited with good composition fidelity even if not in a crystalline phase. All coatings are nanostructured and non-cytotoxic and display variable surface roughness and wettability. Upon heating, higher adhesion and hydrophilicity are obtained as well as higher stability, resulting in better cell viability. Interestingly, different phosphates show very different in vitro behavior, with brushite being the most suitable for promoting cell viability and beta-tricalcium phosphate having a higher impact on cell morphology at the early timepoints. [ABSTRACT FROM AUTHOR]

Brushite coatings were obtained on titanium by the method of electrochemical deposition from Ca(NO3)2/NH4H2PO4 electrolyte at Ca/P = 1.67, pH 4, and a constant voltage of 15 V or a current density of 20 mA/cm2 for 20 min. In a medium of 0.01–0.10% polyvinyl alcohol at a constant voltage of 15 V, single-phase brushite or monetite coatings are deposited. The addition of 0.01–0.10% polyvinyl alcohol to the electrolyte during deposition at a constant current density of 20 mA/cm2 leads to the formation of composite calcium phosphate coatings containing brushite, calcium hydroxide, and calcium phosphate of the apatite structure. The bioactivity of calcium phosphate coatings was confirmed by the formation of apatites during their soaking in the Simulated Body Fluid (SBF). Amorphized apatite that formed on brushite coatings during soaking for 2 weeks in SBF crystallizes into β-tricalcium phosphate after heat treatment. The apatite that formed on the composite coating in the SBF crystallizes into a composition of hydroxyapatite and β-tricalcium phosphate. The resulting bioactive calcium phosphate coatings can be used as biocoatings to enhance osseointegration of titanium implants. [ABSTRACT FROM AUTHOR]

The influence of ionic substitution in the Ca1−xCoxHPO4·nH2O compound was studied systematically for the first time. Among the fascinating features of these biomaterials is that they can be easily tailored for specific applications, for example, as biocements and bioceramics. Different molar concentrations of Co(NO3)2·6H2O, Ca(NO3)2·4H2O, and NaH2PO4·2H2O compounds were employed in determining the starting solutions utilized in the present study. The experimental findings reveal that, when the Co/Ca molar ratio is below 0.67 (BCo4), Co doping (the partial substitution of Ca by Co) takes place in brushite as a monophase. However, in the Co/Ca 0.67–1.5 molar ratio range (BCo4–BCo6), biphasic Co3(PO4)2·8H2O/CaHPO4·2H2O crystals start to precipitate. Full Ca replacement by Co results in the precipitation of nanostructured monoclinic cobalt phosphate and orthorhombic ammonium cobalt phosphate hydrate. Subsequent X-ray photoelectron spectroscopy (XPS), powdered X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) analyses, along with thermogravimetric analysis (TGA), confirmed that the starting solution ratio of Co/Ca had a significant influence on the material's microstructure, while tuning this ratio ultimately tailored the desired properties of the material for the intended applications. [ABSTRACT FROM AUTHOR]

Bioactive calcium phosphate ceramics (CaPs) are one of the building components of the inorganic part of bones. Synthetic CaPs are frequently used as materials for filling bone defects in the form of pastes or composites; however, their porous structure allows modification with active substances and, thus, subsequent use as a drug carrier for the controlled release of active substances. In this study, four different ceramic powders were compared: commercial hydroxyapatite (HA), TCP, brushite, as well as HA obtained by wet precipitation methods. The ceramic powders were subjected to physicochemical analysis, including FTIR, XRD, and determination of Ca/P molar ratio or porosity. These techniques confirmed that the materials were phase-pure, and the molar ratios of calcium and phosphorus elements were in accordance with the literature. This confirmed the validity of the selected synthesis methods. CaPs were then modified with the antibiotic clindamycin. Drug release was determined on HPLC, and antimicrobial properties were tested against Staphylococcus aureus. The specific surface area of the ceramic has been demonstrated to be a factor in drug release efficiency. [ABSTRACT FROM AUTHOR]

Microporous ceramic material, based on β-tricalcium phosphate β-Ca3(PO4)2 with grain size 2–5 μm, pore size smaller than 10 mm, and density 1.22 g/cm3 corresponding to ~40% of the theoretical density (3.07 g/cm3) of β-Ca3(PO4)2, was obtained from a powder mixture with a given molar ratio Ca/P = 1.5 after firing at 1100 °C. A homogenized powder mixture of synthetic dicalcium hydrogen phosphates with the molar ratio Ca/P = 1 and calcium citrate tetrahydrate Ca3(C6H5O7)2·4H2O with the molar ratio Ca/P = ∞ was used for microporous ceramic preparation. The phase composition of calcium phosphate powder, synthesized from an aqueous solution of phosphoric acid H3PO4 and calcium carbonate CaCO3 powder, included brushite CaHPO4·2H2O as the predominant phase. Formation of β-tricalcium phosphate β-Ca3(PO4)2 during firing occurred due to the heterophase interaction of the products of thermal decomposition of the components of the starting powder mixture, namely, calcium pyrophosphate Ca2P2O7 and calcium oxide CaO. The formation of arch-like structures from β-tricalcium phosphate β-Ca3(PO4)2 grains, which were tightly sintered together, hindered the shrinkage of ceramics. The microporous ceramics obtained, based on β-tricalcium phosphate β-Ca3(PO4)2, can be recommended as a biocompatible and biodegradable material for treatment of bone defects and as a substrate for bone-cell cultivation.

Calcium phosphate composite powders consisting of brushite and calcite were obtained in an aqueous medium from a CaCO3/Ca(H2PO4)2 suspension at Ca/P ratios of 1,33, 1,50, 1,67, pH 5–7, and maturation time of 21-50 days. Prolonged maturation (up to 68 days) of composite calcium phosphate powders led to a hydrolytic transition of brushite to octacalcium phosphate, the amount of which increased with increasing duration of the maturation stage. Drying calcium phosphate powders at 37°C for 24 h contributed to the partially transition of the metastable phase of octacalcium phosphate to apatite represented by amorphous calcium phosphate. The presence of vibrations of О–Н at 633 cm-1 as the shoulder on the IR spectra indicates the presence of apatite in calcium phosphate powders. The use of an electric current (20 mA/cm2, 3–20 min) for a local increase of the pH value made it possible to increase the amount of octacalcium phosphate in the composition of the composite powder, which has a characteristic rosette morphology of thin lamellar crystallites.

Objective: A triphasic bone graft block composed of gypsum, brushite, and monetite is expected to be better for regenerating bone than a gypsum-hydroxyapatite-tricalcium phosphate block. Therefore, the aim of this study was to fabricate and evaluate the mechanical properties of a newly developed triphasic block composed of gypsum, brushite, and monetite. Materials and method: Triphasic blocks were prepared by mixing calcium sulfate hemihydrate, brushite, and monetite powders with distilled water at a powder-to-liquid ratio of 0.5. The content of calcium sulfate hemihydrate was fixed at 50%, and the contents of brushite and monetite powders were varied. After molding and setting, the obtained blocks were characterized, and their mechanical properties were evaluated. Results: The triphasic blocks were prepared and could maintain their shape without collapsing. The XRD characterization of the obtained triphasic blocks showed that only three phases existed in the block. Calcium sulfate hemihydrate was transformed into its dihydrate form and provided mechanical strength to the block through a setting mechanism. The transformation of calcium sulfate hemihydrate into its dihydrate crystals formed an interlocked structure that was disrupted in triphasic blocks, as observed in SEM images. The disruption of the interlocked structure resulted in lower mechanical strength of the obtained triphasic blocks compared to the set gypsum control. The variation in brushite and monetite composition did not affect the mechanical properties of the triphasic blocks. Conclusion: The triphasic gypsum-brushite-monetite block was successfully prepared, and no other crystal phases were found. The triphasic blocks could maintain their shape after setting. The addition of brushite and monetite powders disrupted the interlocked structure of the set gypsum crystal, resulting in a decrease in mechanical strength. Furthermore, the variation in brushite and monetite powders did not affect the mechanical properties of the triphasic blocks.

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 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. [ABSTRACT FROM AUTHOR]

Fine powders of brushite CaHPO4·2H2O, ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O), and calcium sulfate dihydrate CaSO4·2H2O—all containing sodium chloride NaCl as a reaction by-product—were synthesized from 0.5 M aqueous solution of calcium chloride CaCl2, sodium hydrophosphate Na2HPO4 and/or sodium sulfate Na2SO4. Powder of ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O) was synthesized by precipitation from aqueous solution of calcium chloride CaCl2 and mixed-anionic solution simultaneously containing the hydrogen phosphate anion HPO42− (Na2HPO4) and sulfate anion SO42− (Na2SO4). Sodium chloride NaCl, presenting in compacts based on synthesized powders of brushite CaHPO4·2H2O, ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O) and calcium sulfate dihydrate CaSO4·2H2O, was responsible for both low-temperature melt formation and the creation of phase composition of ceramics. Heterophase interaction of components led to the resulting phase composition of the ceramic samples during heating, including the formation of chlorapatite Ca5(PO4)3Cl in powders of brushite and ardealite. The phase composition of the ceramics based on the powder of brushite CaHPO4·2H2O containing NaCl as a by-product after firing at 800–1000 °C included β-Ca2P2O7, and Ca5(PO4)3Cl. The phase composition of ceramics based on the powder of ardealite Ca(HPO4)x(SO4)1−x·2H2O (Ca(HPO4)0.5(SO4)0.5·2H2O) containing NaCl as a by-product after firing at 800 and 900 °C included β-Ca2P2O7, CaSO4, and Ca5(PO4)3Cl; after firing at 1000 °C, it includedCaSO4, Ca5(PO4)3Cl and Ca3(PO4)2/Ca10Na(PO4)7, and after firing at 1100 °C, it included CaSO4 and Ca5(PO4)3Cl. The phase composition of ceramics based on powder of calcium sulfate dihydrate CaSO4·2H2O containing NaCl as a by-product after firing at 800–1100 °C included CaSO4 as the predominant phase. The phase composition of all ceramic samples under investigation consisted of biocompatible crystalline phases with different abilities to biodegrade. For this reason, the created ceramics can be recommended for testing as materials for treatment of bone defects using regenerative medicine methods. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Calcium phosphate (CaP) with several chemical compositions and morphologies was prepared by precipitation using aqueous solutions of L-Glutamic acid (H2G) and calcium hydroxide, both mixed together with an aqueous solution (0.15 M) of phosphoric acid. Plate-shaped dicalcium phosphate dihydrate (brushite) particles were obtained and identified at a lower concentration of the solution of the reactants. The Ca/P ratio deduced by EDS was ~1, as expected. The nanoscale dimension of carbonate apatite and amorphous calcium phosphate, with variable Ca/P ratios, were revealed by X-ray diffraction (XRD) and scanning electron microscopy and energy dispersive X-ray spectroscopy analysis (SEM-EDS). They were characterized in medium and high concentrations of calcium hydroxide (0.15 M and 0.20 M). The equilibria involved in all the reactions in aqueous solution were determined. The thermodynamic calculations showed a decrease in the amount of chelate complexes with an increase in pH, being the opposite of [CaPO4−] and [CaHG+]. This fluctuation showed an evident influence on the morphology and polymorphism of CaP particles obtained under the present experimental conditions, with potential use as a biomaterial. [ABSTRACT FROM AUTHOR]

Synthesis from mixed-anionic aqueous solutions is a novel approach to obtain active powders for bioceramics production in the CaO-SiO2-P2O5-Na2O system. In this work, powders were prepared using precipitation from aqueous solutions of the following precursors: Ca(NO3)2 and Na2HPO4 (CaP); Ca(NO3)2 and Na2SiO3 (CaSi); and Ca(NO3)2, Na2HPO4 and Na2SiO3 (CaPSi). Phase composition of the CaP powder included brushite CaHPO4‧2H2O and the CaSi powder included calcium silicate hydrate. Phase composition of the CaPSi powder consisted of the amorphous phase (presumably containing hydrated quasi-amorphous calcium phosphate and calcium silicate phase). All synthesized powders contained NaNO3 as a by-product. The total weight loss after heating up to 1000 °C for the CaP sample—28.3%, for the CaSi sample—38.8% and for the CaPSi sample was 29%. Phase composition of the ceramic samples after the heat treatment at 1000 °C based on the CaP powder contained β-NaCaPO4 and β-Ca2P2O7, the ceramic samples based on the CaSi powder contained α-CaSiO3 and Na2Ca2Si2O7, while the ceramics obtained from the CaPSi powder contained sodium rhenanite β-NaCaPO4, wollastonite α-CaSiO3 and Na3Ca6(PO4)5. The densest ceramic sample was obtained in CaO-SiO2-P2O5-Na2O system at 900 °C from the CaP powder (ρ = 2.53 g/cm3), while the other samples had densities of 0.93 g/cm3 (CaSi) and 1.22 (CaPSi) at the same temperature. The ceramics prepared in this system contain biocompatible and bioresorbable phases, and can be recommended for use in medicine for bone-defect treatment. [ABSTRACT FROM AUTHOR]

In recent years, significant developments have taken place in scientific fields such as tissue and materials engineering, which allow for the development of new, intelligent biomaterials. An example of such biomaterials is drug delivery systems that release the active substance directly at the site where the therapeutic effect is required. In this research, polymeric materials and ceramic–polymer composites were developed as carriers for the antibiotic clindamycin. The preparation and characterization of biomaterials based on hyaluronic acid, collagen, and nano brushite obtained using the photocrosslinking technique under UV (ultraviolet) light are described. Physical and chemical analyses of the materials obtained were carried out using Fourier transform infrared spectroscopy (FT-IR) and optical microscopy. The sorption capacities were determined and subjected to in vitro incubation in simulated biological environments such as Ringer’s solution, simulated body fluid (SBF), phosphate-buffered saline (PBS), and distilled water. The antibiotic release rate was also measured. The study confirmed higher swelling capacity for materials with no addition of a ceramic phase, thus it can be concluded that brushite inhibits the penetration of the liquid medium into the interior of the samples, leading to faster absorption of the liquid medium. In addition, incubation tests confirmed preliminary biocompatibility. No drastic changes in pH values were observed, which suggests that the materials are stable under these conditions. The release rate of the antibiotic from the biomaterial into the incubation medium was determined using high-pressure liquid chromatography (HPLC). The concentration of the antibiotic in the incubation fluid increased steadily following a 14-day incubation in PBS, indicating continuous antibiotic release. Based on the results, it can be concluded that the developed polymeric material demonstrates potential for use as a carrier for the active substance.

This study aimed to explore the effects of the full-scale replacement (up to 100%) of Ca2+ ions with Ag1+ ions in the structure of brushite (CaHPO4·2H2O). This substitution has potential benefits for producing monophasic and biphasic Ca1−xAgxHPO4·nH2O compounds. To prepare the starting solutions, (NH4)2HPO4, Ca(NO3)2·4H2O, and AgNO3 at different concentrations were used. The results showed that when the Ag/Ca molar ratio was below 0.25, partial substitution of Ca with Ag reduced the size of the unit cell of brushite. As the Ag/Ca molar ratio increased to 4, a compound with both monoclinic CaHPO4·2H2O and cubic nanostructured Ag3PO4 phases formed. There was a nearly linear relationship between the Ag ion ratio in the starting solutions and the wt% precipitation of the Ag3PO4 phase in the resulting compound. Moreover, when the Ag/Ca molar ratio exceeded 4, a single-phase Ag3PO4 compound formed. Hence, adjusting the Ag/Ca ratio in the starting solution allows the production of biomaterials with customized properties. In summary, this study introduces a novel synthesis method for the mono- and biphasic Ca1−xAgxHPO4·nH2O compounds brushite and silver phosphate. The preparation of these phases in a one-pot synthesis with controlled phase composition resulted in the enhancement of existing bone cement formulations by allowing better mixing of the starting ingredients.

A triphasic bone graft block composed of gypsum, brushite, and monetite is expected to be better for regenerating bone than a gypsum-hydroxyapatite-tricalcium phosphate block. Therefore, the aim of this study was to fabricate and evaluate the mechanical properties of a newly developed triphasic block composed of gypsum, brushite, and monetite. Triphasic blocks were prepared by mixing calcium sulfate hemihydrate, brushite, and monetite powders with distilled water at a powder-to-liquid ratio of 0.5. The content of calcium sulfate hemihydrate was fixed at 50%, and the contents of brushite and monetite powders were varied. After molding and setting, the obtained blocks were characterized, and their mechanical properties were evaluated. The triphasic blocks were prepared and could maintain their shape without collapsing. The XRD characterization of the obtained triphasic blocks showed that only three phases existed in the block. Calcium sulfate hemihydrate was transformed into its dihydrate form and provided mechanical strength to the block through a setting mechanism. The transformation of calcium sulfate hemihydrate into its dihydrate crystals formed an interlocked structure that was disrupted in triphasic blocks, as observed in SEM images. The disruption of the interlocked structure resulted in lower mechanical strength of the obtained triphasic blocks compared to the set gypsum control. The variation in brushite and monetite composition did not affect the mechanical properties of the triphasic blocks. The triphasic gypsum-brushite-monetite block was successfully prepared, and no other crystal phases were found. The triphasic blocks could maintain their shape after setting. The addition of brushite and monetite powders disrupted the interlocked structure of the set gypsum crystal, resulting in a decrease in mechanical strength. Furthermore, the variation in brushite and monetite powders did not affect the mechanical properties of the triphasic blocks. [ABSTRACT FROM AUTHOR]

Microporous ceramic material, based on β-tricalcium phosphate β-Ca3(PO4)2 with grain size 2–5 μm, pore size smaller than 10 mm, and density 1.22 g/cm3 corresponding to ~40% of the theoretical density (3.07 g/cm3) of β-Ca3(PO4)2, was obtained from a powder mixture with a given molar ratio Ca/P = 1.5 after firing at 1100 °C. A homogenized powder mixture of synthetic dicalcium hydrogen phosphates with the molar ratio Ca/P = 1 and calcium citrate tetrahydrate Ca3(C6H5O7)2·4H2O with the molar ratio Ca/P = ∞ was used for microporous ceramic preparation. The phase composition of calcium phosphate powder, synthesized from an aqueous solution of phosphoric acid H3PO4 and calcium carbonate CaCO3 powder, included brushite CaHPO4·2H2O as the predominant phase. Formation of β-tricalcium phosphate β-Ca3(PO4)2 during firing occurred due to the heterophase interaction of the products of thermal decomposition of the components of the starting powder mixture, namely, calcium pyrophosphate Ca2P2O7 and calcium oxide CaO. The formation of arch-like structures from β-tricalcium phosphate β-Ca3(PO4)2 grains, which were tightly sintered together, hindered the shrinkage of ceramics. The microporous ceramics obtained, based on β-tricalcium phosphate β-Ca3(PO4)2, can be recommended as a biocompatible and biodegradable material for treatment of bone defects and as a substrate for bone-cell cultivation. [ABSTRACT FROM AUTHOR]

Herein, pyrite‐leaching liquid and naringin‐loaded microspheres are incorporated into brushite to prepare composite scaffolds with enhanced osteogenic properties in vitro for bone tissue engineering. The results reveal that the loading of these two medicines has no significant effect on the crystalline phase of the composite, while some changes happen to the chemical groups when the dosage of the microspheres is controlled within 1.5 wt%. After soaking in phosphate buffer for 24 days, the composite containing 0%, 0.38 wt%, 0.75 wt%, and 1.50 wt% naringin‐loaded microspheres show a weight loss rate of 19.28%, 18.81%, 16.92%, and 14.14%, respectively. Simultaneously, the soaking assay reveals that the release of naringin and Fe are both kept within a safe level. A burst release of naringin is avoided since the highest concentration of naringin is detected on day 12 after immersion. The cell experiments show that all the composites have no toxicity to osteoblasts and allow the cells to grow on the surface. Furthermore, adding naringin‐loaded microspheres to the composite (0.75–1.5 wt%) promotes the mineralization ability and the alkaline phosphatase activity of the osteoblasts. Thus, the novel pyrite/naringin/brushite composite scaffold has the potential to be used in bone tissue engineering. [ABSTRACT FROM AUTHOR]

β-Tricalcium phosphate (β-Ca3(PO4)2) based ceramics with a relative density of 20–21%, grain size from 200 to 600 nm, and compressive strength from 1.6 to 1.8 MPa have been produced by 1000°C firing of cement stone prepared from a powder mixture having a Ca/P molar ratio of 1.5 and consisting of hydroxyapatite (Ca10(PO4)6(OH)2), calcium citrate tetrahydrate (Ca3(C6H5O7)2·4H2O), and calcium dihydrogen phosphate monohydrate (Ca(H2PO4)2·H2O). The mixing liquid used to initiate chemical binding reaction in the powder mixture was distilled water. The phase composition of the cement stone included brushite (CaHPO4·2H2O) and unreacted starting materials. The presence of platelike calcium pyrophosphate (Ca2P2O7) particles, formed from platelike brushite (CaHPO4·2H2O) particles, impeded densification of the ceramics during firing and ensured the formation of an ultraporous structure. The submicron-grained microstructure and phase composition of the β-Ca3(PO4)2-based ceramics resulted mainly from heterophase interactions between the products of thermal decomposition of cement stone components. Offering sufficient strength, biocompatible and bioresorbable ultraporous submicron-grained β-Ca3(PO4)2-based ceramics can be recommended for use in regenerative medicine for bone tissue defect repair. [ABSTRACT FROM AUTHOR]

The present investigation exposes the main results raised from an active collaboration started in 2018 with the San Pio Hospital (Benevento, Southern Italy), aiming at a detailed mineralogical investigation of urinary stones of patients from the Campania region. Forty-nine uroliths (both bladder and kidney stones) have been surgically collected from patients admitted between 2018 and 2020 at the Department of Urology of the San Pio Hospital and characterized for clinical purposes and environmental biomonitoring from a mineralogical point of view. Possible causes and environmental implications were inferred according to the morpho-constitutional classification of the uroliths carried out by means of a conventional analytical approach. The mineralogical frequency distribution of uroliths from the Campanian region can be discussed as a function of dietary, socio-demographic, and environmental risk factors. Whewellite [CaC2O4·H2O] and weddellite [CaC2O4·(2+x)H2O], along with anhydrous calcium oxalate, represent the main mineralogical phases forming the biominerals examined here. Worth to note is that the percentage of oxalates in the Campanian region (ca. 51%) is quite comparable to those of other Mediterranean areas. Frequent uricite [C5H4N4O3] (ca. 33%), mainly observed in bladder stones of older male patients, could be related to an incorrect lifestyle and dietary habits. Occurrence of lower percentages of phosphate (i.e., brushite [CaHPO4·2(H2O)] and carbonated apatite [Ca10(PO4CO3)6(OH)8]) and mixed stones (such as, for example, a mixture of ammonium urate [NH4C5H3N4O3] and calcium oxalates) indicates specific etiopathogenetic mechanisms, suggesting proper therapeutical approaches. [ABSTRACT FROM AUTHOR]

Recently, synthetic magnesium whitlockite (Ca 18 Mg 2 (HPO 4) 2 (PO 4) 12 , WH) has received much attention for being used as a bone substitute. The present research explores the possibility of tailoring Ca to Mg ratio in WH structure material, which might subsequently affect its biological properties. A dissolution-precipitation synthesis of nanocrystalline WH samples was performed at 65 °C using brushite as a starting material in the presence of Mg2+ ions. The change in the stoichiometry of synthesized samples was reflected in the variation of lattice parameters: the decrement of crystallographic constants was attributed to the difference in ionic radius of Ca and Mg ions. The synthesized powders were characterized to determine the phase purity, crystallographic parameters, functional groups, and morphology under altered Ca to Mg molar ratios. [ABSTRACT FROM AUTHOR]

The effect of Ca2+ amount and sintering temperature on mechanical properties of geopolymer-brushite (GPB) binders was investigated. Brushite and raw abandoned kaolinite clay thermally transformed into metakaolin were used for GPB synthesis. The complete phase and structural analyses were performed by X-ray powder diffraction, and Fourier transforms infrared spectroscopy (FT-IR). The pore-filling effect as a consequence of Ca2+ ions incorporation into the hybrid geopolymer networks improved the compressive strength. On the other hand, the chosen biscuit sintering at 800 and 900oC caused the phase transformation of brushite into calcium pyrophosphate, which negatively affected the compressive strength of such materials. The obtained results indicate that the usage of relatively high sintering temperatures is not always the necessary step for producing geopolymer-based types of cement with prominent mechanical properties.

Brushite, or Dicalcium phosphate dihydrate (CaHPO 4 ·2H 2 O), is a well-known calcium phosphate (CaP) found in mineralized tissues and is utilized in medical treatment, particularly in bone powder for bone repair. Brushites with Zn2+ and Ag + ions concentration were synthesized in an aqueous solution using the conventional precipitation procedure. The synthesized brushites were characterized using techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction (PXRD), Scanning Electron Microscopy (SEM), and bioassays were carried out to evaluate their antibacterial and antifungal activities. The alterations in PXRD and FTIR peak locations demonstrated that zinc and silver ions were effectively inserted into the brushite crystals. Initial tests revealed that the powders were innocuous, which make them potentially beneficial for mineralized tissue engineering. These brushites exhibited remarkable antimicrobial activities. Zn-doped brushite completely controlled the growth of fungi namely Macrophomina phaseolina and Sclerotium rolfsii at a concentration of 0.0039 mg mL−1 while Ag-doped brushite completely arrested the growth of these fungi at 0.0312 and 0.0039 mg mL−1, respectively. Likewise, both the brushite exhibited remarkable antibacterial activity against Bacillus thuringiensis and moderate activity against Escherichia coli. Brushite compounds coupled with active metal ions, notably Ag+ and Zn2+, demonstrated promise as a distinct class of reactive materials for bone-related applications. • Metal-Doped Brushite Powder with controlled particle properties was rapidly synthesized using a coprecipitation method. • The obtained powders were physically characterized using different techniques (SEM, PXRD, FTIR, and DLS). • The results showed significant level of antimicrobial activity against different bacterial and fungal strains. • Metal doped Brushite proved highly antifungal and could be considered as reactive CaPs for bone regeneration applications. [ABSTRACT FROM AUTHOR]

This study examined the profile of patients and the impact of diet on the risk of brushite stone formation under controlled, standardized conditions. Sixty-five patients with brushite nephrolithiasis were enrolled in the study. Metabolic, dietary, and 24 h urinary parameters were collected under the habitual, self-selected diet of the patients and the balanced mixed, standardized diet. The [13C2]oxalate absorption, ammonium chloride, and calcium loading tests were conducted. All patients had at least one abnormality on the usual diet, with hypercalciuria (84.6%), increased urine pH (61.5%), and hyperphosphaturia (43.1%) being the most common. Absorptive hypercalciuria was present in 32.1% and hyperabsorption of oxalate in 41.2%, while distal renal tubular acidosis (dRTA) was noted in 50% of brushite stone formers. The relative supersaturation of brushite did not differ between patients with and without dRTA. Among all recent brushite-containing calculi, 61.5% were mixed with calcium oxalate and/or carbonate apatite. The relative supersaturation of brushite, apatite, and calcium oxalate decreased significantly under the balanced diet, mainly due to the significant decline in urinary calcium, phosphate, and oxalate excretion. Dietary intervention was shown to be effective and should be an integral part of the treatment of brushite stone disease. Further research on the role of dRTA in brushite stone formation is needed.

This study was carried out to investigate the effect of a complete exchange of Ca2+ with Zn2+ ions on the structure of brushite (CaHPO4·2H2O), which might be advantageous in the production process of CaxZn1−xHPO4·nH2O. To acquire the starting solutions needed for the current study, (NH4)2HPO4, Ca(NO3)2·4H2O, and Zn(NO3)2·6H2O were utilized in several molar concentrations. The findings indicate that Ca is partly substituted by Zn when the Zn/Ca molar ratio is below 0.25 and that Zn doping hinders the crystallization of brushite. A continued increase in the Zn/Ca molar ratio to 1 (at which point the supersaturation of the Zn solution rises) led to a biphasic compound of monoclinic brushite and parascholzite precipitate. Elevating the Zn/Ca molar ratio to 1.5 resulted in a precipitate of a parascholzite-like mineral. Finally, increasing the Zn/Ca molar ratio to 4 and above resulted in the formation of the hopeite mineral. Future biomaterial production with specific and bespoke characteristics can be achieved by adjusting the Zn/Ca ratio in the starting solution. It Rhas been established that the Zn/Ca ratio in the starting solution can be adjusted to obtain minerals with specific compositions. Thus, new synthesis methods for parascholzite and hopeite were introduced for the first time in this manuscript.

Calcium phosphate coatings on titanium plates were obtained by electrochemical deposition at room temperature in a two-electrode cell at a constant current density of 30 mA/sm^2 and a deposition time of 10 min, and brushite coatings from Ca(NO3)2 / NH4H2PO4 system at pH=4, and composite (brushite/calcite/apatite) coatings from the CаCO3 / Ca(H2PO4)2 system at pH=5. The apatite-forming ability (bioactivity) was determined by soaking both types of calcium phosphate coatings in a model SBF solution during month. The newly formed amorphized apatite layer after heat treatment at 800°С crystallized into β–tricalcium phosphate/hydroxyapatite on brushite coatings and hydroxyapatite on composite coatings due to the presence of calcite, whose carbonate ions initiate formation of hydroxyapatite, as well as apatite nanoparticles in the initial coating. The obtained calcium phosphate coatings are promising as biocoatings capable to increase osseointegration of metal implants.

Hydroxyapatite (HA) nanopowders are attracting interest for surface application to ceramic biomaterials. In this study, we developed innovative and new viable synthesis routes of calcium phosphate nanopowders from the natural calcium carbonate of chicken eggshells. Following the four routes, alternative co-precipitation, vacuum process, brushite, and calcination, we obtained the HA samples, which were then characterized by different methods. The X-ray diffraction /Rietveld method showed the HA phases, monetite and brushite crystallinity with greater symmetry, and nanoscale. Transmission electron microscopy showed the morphology of nanoparticles functionalized nanoparticles smaller than 100 nm in routes A, B and D, and Fourier-transform infrared spectrophotometry and Raman spectroscopy identified the classic chemical groups of calcium phosphates by four routes mainly groups (PO4)3- and (CO3-). Scanning electron microscopy analysis revealed a good surface topography to future cell biointeraction in A, B and D routes, and thermogravimetric analysis showed the mass loss profile inherent to each synthesis route with slot at 200 °C. Hence, the eggshell HA and brushite and the specific monetite nanoparticles with different morphology can be prepared from the four new possible and viable routes using different methods.