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Sample records for brushite calcium phosphate

  1. Frozen delivery of brushite calcium phosphate cements.

    Science.gov (United States)

    Grover, Liam M; Hofmann, Michael P; Gbureck, Uwe; Kumarasami, Balamurgan; Barralet, Jake E

    2008-11-01

    Calcium phosphate cements typically harden following the combination of a calcium phosphate powder component with an aqueous solution to form a matrix consisting of hydroxyapatite or brushite. The mixing process can be very important to the mechanical properties exhibited by cement materials and consequently when used clinically, since they are usually hand-mixed their mechanical properties are prone to operator-induced variability. It is possible to reduce this variability by pre-mixing the cement, e.g. by replacing the aqueous liquid component with non-reactive glycerol. Here, for the first time, we report the formation of three different pre-mixed brushite cement formulations formed by freezing the cement pastes following combination of the powder and liquid components. When frozen and stored at -80 degrees C or less, significant degradation in compression strength did not occur for the duration of the study (28 days). Interestingly, in the case of the brushite cement formed from the combination of beta-tricalcium phosphate with 2 M orthophosphoric acid solution, freezing the cement paste had the effect of increasing mean compressive strength fivefold (from 4 to 20 MPa). The increase in compression strength was accompanied by a reduction in the setting rate of the cement. As no differences in porosity or degree of reaction were observed, strength improvement was attributed to a modification of crystal morphology and a reduction in damage caused to the cement matrix during manipulation.

  2. In vitro ageing of brushite calcium phosphate cement.

    Science.gov (United States)

    Grover, L M; Knowles, J C; Fleming, G J P; Barralet, J E

    2003-10-01

    In vivo studies investigating the use of brushite cements have demonstrated mixed results with one or more of dissolution, hydrolysis, fragmentation and long term stability being demonstrated. It has been suggested that sample volume, implant location, and species can affect in vivo behaviour. As few in vitro studies on this cement system have been performed, this study aimed to compare the effects of static and dynamic in vitro ageing protocols on the phase composition, weight loss and mechanical properties of brushite cement. The effects of immersion liquid to cement volume ratio (LCVR) and sample volume on phase composition were investigated and comparative in vitro experiments were also performed in foetal bovine serum. It was determined that the weight loss after 28 days was up to seven times higher in serum than in phosphate buffered saline (PBS) and that fragmentation accounted for most of the weight loss observed. Hydroxyapatite was formed in PBS but not in serum when aged in refreshed media at all LCVRs investigated. This study has highlighted that LCVR, media refresh rate and media composition are critical to brushite cement performance. It appears that brushite cement removal from an implant site may be complex and dependent on physiological processes other than simple dissolution. A better understanding of these processes could provide the means to engineer more precise calcium phosphate cement degradation profiles.

  3. Biocompatibility and resorption of a brushite calcium phosphate cement.

    Science.gov (United States)

    Theiss, Felix; Apelt, Detlef; Brand, Bastian; Kutter, Annette; Zlinszky, Katalin; Bohner, Marc; Matter, Sandro; Frei, Christian; Auer, Joerg A; von Rechenberg, Brigitte

    2005-07-01

    A hydraulic calcium phosphate cement with beta-tricalcium phosphate (TCP) granules embedded in a matrix of dicalcium phosphate dihydrate (DCPD) was implanted in experimentally created defects in sheep. One type of defect consisted of a drill hole in the medial femoral condyle. The other, partial metaphyseal defect was located in the proximal aspect of the tibia plateau and was stabilized using a 3.5 mm T-plate. The bone samples of 2 animals each per group were harvested after 2, 4, 6 and 8 weeks. Samples were evaluated for cement resorption and signs of immediate reaction, such as inflammation, caused by the cement setting in situ. Differences regarding these aspects were assessed for both types of defects using macroscopical, radiological, histological and histomorphometrical evaluations. In both defects the brushite matrix was resorbed faster than the beta-TCP granules. The resorption front was followed directly by a front of new bone formation, in which residual beta-TCP granules were embedded. Cement resorption occurred through (i) extracellular liquid dissolution with cement disintegration and particle formation, and (ii) phagocytosis of the cement particles through macrophages. Signs of inflammation or immunologic response leading to delayed new bone formation were not noticed at any time. Cement degradation and new bone formation occurred slightly faster in the femur defects.

  4. Brushite-based calcium phosphate cement with multichannel hydroxyapatite granule loading for improved bone regeneration.

    Science.gov (United States)

    Sarkar, Swapan Kumar; Lee, Byung Yeol; Padalhin, Andrew Reyas; Sarker, Avik; Carpena, Nathaniel; Kim, Boram; Paul, Kallyanshish; Choi, Hwan Jun; Bae, Sang-Ho; Lee, Byong Taek

    2016-01-01

    In this work, we report brushite-based calcium phosphate cement (CPC) system to enhance the in vivo biodegradation and tissue in-growth by incorporation of micro-channeled hydroxyapatite (HAp) granule and silicon and sodium addition in calcium phosphate precursor powder. Sodium- and silicon-rich calcium phosphate powder with predominantly tri calcium phosphate (TCP) phase was synthesized by an inexpensive wet chemical route to react with mono calcium phosphate monohydrate (MCPM) for making the CPC. TCP nanopowder also served as a packing filler and moderator of the reaction kinetics of the setting mechanism. Strong sintered cylindrical HAp granules were prepared by fibrous monolithic (FM) process, which is 800 µm in diameter and have seven micro-channels. Acid sodium pyrophosphate and sodium citrate solution was used as the liquid component which acted as a homogenizer and setting time retarder. The granules accelerated the degradation of the brushite cement matrix as well as improved the bone tissue in-growth by permitting an easy access to the interior of the CPC through the micro-channels. The addition of micro-channeled granule in the CPC introduced porosity without sacrificing much of its compressive strength. In vivo investigation by creating a critical size defect in the femur head of a rabbit model for 1 and 2 months showed excellent bone in-growth through the micro-channels. The granules enhanced the implant degradation behavior and bone regeneration in the implanted area was significantly improved after two months of implantation.

  5. In vitro biodegradation of three brushite calcium phosphate cements by a macrophage cell-line.

    Science.gov (United States)

    Xia, Zhidao; Grover, Liam Michael; Huang, Yizhong; Adamopoulos, Iannis E; Gbureck, Uwe; Triffitt, James T; Shelton, Richard M; Barralet, Jake E

    2006-09-01

    Depending upon local conditions, brushite (CaHPO4 x 2 H2O) cements may be largely resorbed or (following hydrolysis to hydroxyapatite) remain stable in vivo. To determine which factors influence cement resorption, previous studies have investigated the solution-driven degradation of brushite cements in vitro in the absence of any cells. However, the mechanism of cell-mediated biodegradation of the brushite cement is still unknown. The aim of the current study was to observe the cell-mediated biodegradation of brushite cement formulations in vitro. The cements were aged in the presence of a murine cell line (RAW264.7), which had the potential to form osteoclasts in the presence of the receptor for nuclear factor kappa B ligand (RANKL) in vitro, independently of macrophage colony stimulating factor (M-CSF). The cytotoxicity of the cements on RAW264.7 cells and the calcium and phosphate released from materials to the culture media were analysed. Scanning electron microscopy (SEM) and focused ion beam (FIB) microscopy were used to characterise the ultrastructure of the cells. The results showed that the RAW264.7 cell line formed multinucleated TRAP positive osteoclast-like cells, capable of ruffled border formation and lacunar resorption on the brushite calcium phosphate cement in vitro. In the osteoclast-like cell cultures, ultrastructural analysis by SEM revealed phenotypic characteristics of osteoclasts including formation of a sealing zone and ruffled border. Penetration of the surface of the cement, was demonstrated using FIB, and this showed the potential demineralising effect of the cells on the cements. This study has set up a useful model to investigate the cell-mediated cement degradation in vitro.

  6. Visualising phase change in a brushite-based calcium phosphate ceramic

    Science.gov (United States)

    Bannerman, A.; Williams, R. L.; Cox, S. C.; Grover, L. M.

    2016-09-01

    The resorption of brushite-based bone cements has been shown to be highly unpredictable, with strong dependence on a number of conditions. One of the major factors is phase transformation, with change to more stable phases such as hydroxyapatite affecting the rate of resorption. Despite its importance, the analysis of phase transformation has been largely undertaken using methods that only detect crystalline composition and give no information on the spatial distribution of the phases. In this study confocal Raman microscopy was used to map cross-sections of brushite cylinders aged in Phosphate Buffered Saline, Foetal Bovine Serum, Dulbecco’s – Minimum Essential Medium (with and without serum). Image maps showed the importance of ageing medium on the phase composition throughout the ceramic structure. When aged without serum, there was dissolution of the brushite phase concomitant to the deposition of octacalcium phosphate (OCP) around the periphery of the sample. The deposition of OCP was detectable within five days and reduced the rate of brushite dissolution from the material. The use of serum, even at a concentration of 10vol% prevented phase transformation. This paper demonstrates the value of confocal Raman microscopy in monitoring phase change in biocements; it also demonstrates the problems with assessing material degradation in non-serum containing media.

  7. Ionic modification of calcium phosphate cement viscosity. Part II: hypodermic injection and strength improvement of brushite cement.

    Science.gov (United States)

    Barralet, J E; Grover, L M; Gbureck, U

    2004-05-01

    Brushite-forming calcium phosphate cements are of great interest as bone replacement materials because they are resorbable in physiological conditions. However, their short setting times, low mechanical strengths and limited injectability limit broad clinical application. In this study, we showed that a significant improvement of these properties of brushite cement could be achieved by the use of sodium citrate or citric acid as setting retardants, such that workable cement pastes with a powder to liquid ratio of up to 5 could be manufactured. The cement used in this study consisted of an equimolar powder mixture of beta-tricalcium phosphate and monocalcium phosphate hydrate The use of 500 mM-1M retardant solutions as liquid phase enabled initial setting times of 8-12 min. Wet compressive strength were found to be in the range between 12-18 MPa after immersion of uncompacted cement samples in serum for 24 h. A further strength improvement to 32 MPa was obtained by compaction of the cement paste during samples preparation. This is significant because high-temperature processes cannot be used to fabricate hydrated calcium phosphate materials. Cement pastes were injectable through a hypodermic needle at a powder to liquid ratio of 3.3 g/ml when a 1M citric acid was used as liquid phase, thus enabling precise controlled delivery to small defects.

  8. Kinetics and Isotherm Studies of Copper Removal by Brushite Calcium Phosphate: Linear and Non-Linear Regression Comparison

    OpenAIRE

    2012-01-01

    Interactions of Cu(II) ions with calcium phosphate Brushite (DCPD) in aqueous solutions were investigated by batch conditions and under several sorption parameters like contact time, pH of solution and initial metal concentration. The retention of copper was found maximum and dominated by exchange reaction process in the pH range 4-6. The reaction process was found initially fast and more than 98% was removed at equilibrium. The kinetics data of batch interaction was analyzed with various kin...

  9. The use of brushite calcium phosphate cement for enhancement of bone-tendon integration in an anterior cruciate ligament reconstruction rabbit model.

    Science.gov (United States)

    Wen, Chun-Yi; Qin, Ling; Lee, Kwong-Man; Chan, Kai-Ming

    2009-05-01

    This study was designed to investigate the osteoconductivity and bioresorption of brushite calcium phosphate cement (CPC) in bone-tendon interface healing after anterior cruciate ligament (ACL) reconstruction. Surgical reconstruction using grafted tendon in bone tunnel was performed bilaterally in 28 skeletal mature rabbits. Brushite CPC was implanted between grafted tendon and bone tunnel of one limb with the contralateral one as the control. A batch of 14 rabbits was sacrificed at 6 and 12 weeks, respectively, after surgery. At each time point, six rabbits were used for micro-CT and subsequent histological examinations, whereas the remaining eight rabbits were used for pull-out testing. The components of brushite CPC-dicalcium phosphate dihydrate matrix degraded rapidly with beta-tricalcium phosphate granules left for guiding new bone formation. Brushite CPC augmented the peri-tendon bone volume and promoted bone growth into the healing interface. The ultimate strength and stiffness of the graft-tunnel complexes on experimental side was higher than that of the control by 117% and 102%, respectively, at 6 weeks postoperatively (p brushite CPC caused a paradigm shift in failure mode from intra-tunnel to intra-articular portion at 12 weeks postoperatively (p = 0.013). Brushite CPC significantly enhanced the bone-tendon integration after ACL reconstruction, which provided a scientific basis for clinical application.

  10. Kinetics and Isotherm Studies of Copper Removal by Brushite Calcium Phosphate: Linear and Non-Linear Regression Comparison

    Directory of Open Access Journals (Sweden)

    Adnane El Hamidi

    2012-01-01

    Full Text Available Interactions of Cu(II ions with calcium phosphate Brushite (DCPD in aqueous solutions were investigated by batch conditions and under several sorption parameters like contact time, pH of solution and initial metal concentration. The retention of copper was found maximum and dominated by exchange reaction process in the pH range 4-6. The reaction process was found initially fast and more than 98% was removed at equilibrium. The kinetics data of batch interaction was analyzed with various kinetic models. It was found that the pseudo-first order model using the non-linear regression method predicted best the experimental data. Furthermore, the adsorption process was modeled by Langmuir isotherm and the removal capacity was 331.64 mg.g-1. Consequently, Cu2+ concentration independent kinetics and single surface layer sorption isotherm are then suggested as appropriate mechanisms for the whole process.

  11. Visualising phase change in a brushite-based calcium phosphate ceramic

    OpenAIRE

    2016-01-01

    The resorption of brushite-based bone cements has been shown to be highly unpredictable, with strong dependence on a number of conditions. One of the major factors is phase transformation, with change to more stable phases such as hydroxyapatite affecting the rate of resorption. Despite its importance, the analysis of phase transformation has been largely undertaken using methods that only detect crystalline composition and give no information on the spatial distribution of the phases. In thi...

  12. Urinary supersaturation with respect to brushite in patients suffering calcium oxalate lithiasis.

    Science.gov (United States)

    Berland, Y; Boistelle, R; Olmer, M

    1990-01-01

    The urines of 23 stone-formers presenting repeated calcium oxalate lithiasis and 12 control subjects were collected at six different time periods daily. Supersaturations for calcium oxalate and brushite (DCPD) were calculated using ionic and solubility products. Urines of both groups were supersaturated for calcium oxalate but only urines of the stone-formers were supersaturated for brushite, the most simple calcium phosphate which nucleates very easily at the urinary pH. This fact suggests that the core of the calcium oxalate stone could be made of either a calcium oxalate crystallite or a brushite seed onto which hetergeneous nucleation of calcium oxalate can take place.

  13. Dicalcium phosphate cements: brushite and monetite.

    Science.gov (United States)

    Tamimi, Faleh; Sheikh, Zeeshan; Barralet, Jake

    2012-02-01

    Dicalcium phosphate cements were developed two decades ago and ever since there has been a substantial growth in research into improving their properties in order to satisfy the requirements needed for several clinical applications. The present paper presents an overview of the rapidly expanding research field of the two main dicalcium phosphate bioceramics: brushite and monetite. This review begins with a summary of all the different formulae developed to prepare dicalcium phosphate cements, and their setting reaction, in order to set the scene for the key cement physical and chemical properties, such as compressive and tensile strength, cohesion, injectability and shelf-life. We address the issue of brushite conversion into either monetite or apatite. Moreover, we discuss the in vivo behavior of the cements, including their ability to promote bone formation, biodegradation and potential clinical applications in drug delivery, orthopedics, craniofacial surgery, cancer therapy and biosensors.

  14. Beta-type calcium phosphates with and without magnesium: From hydrolysis of brushite powder to robocasting of periodic scaffolds.

    Science.gov (United States)

    Richard, Raquel C; Sader, Márcia S; Dai, Jisen; Thiré, Rossana M S M; Soares, Gloria D A

    2014-10-01

    Several approaches have attempted to replace extensive bone loss, but each of them has their limitation. Nowadays, additive manufacture techniques have shown great potential for bone engineering. The objective of this study was to synthesize beta tricalcium phosphate (β-TCP), beta tricalcium phosphate substituted by magnesium (β-TCMP), and biphasic calcium phosphate substituted by magnesium (BCMP) via hydrolysis and produce scaffolds for bone regeneration using robocasting technology. Calcium deficient apatites, with and without magnesium were obtained by hydrolysis, calcined and physico-chemically characterized. Colorimetric cell viability assay, calcium nodule formation, and the expression of alkaline phosphatase, osteocalcin, transforming growth factor beta-1 and collagen were assessed using a mouse osteoblastic cell line (MC3T3-E1). Direct-write assembly of cylindrical periodic scaffolds was done via robotic deposition using β-TCP, β-TCMP, and BCMP colloidal inks. The sintered scaffolds were characterized by X-ray diffraction, Fourier-transform infrared spectroscopy, scanning electron microscopy, Archimede's method, and uniaxial compression test. According to the cell viability assay, the powders induced cell proliferation. Calcium nodule formation and bone markers activity suggested that the materials present potential value in bone tissue engineering. The scaffolds built by robocasting presented interconnected porous and exhibited mean compressive strength between 7.63 and 18.67 MPa, compatible with trabecular bone.

  15. The role of hydrogen bonding in the thermal expansion and dehydration of brushite, di-calcium phosphate dihydrate

    Science.gov (United States)

    Schofield, P. F.; Knight, K. S.; Houwen, J. A. M. Van Der; Valsami-Jones, E.

    2004-12-01

    The unit-cell and atomic parameters of perdeuterated brushite have been extracted from Rietveld analysis of neutron powder diffraction data within the temperature range 4.2 to 470 K. The thermal expansion of brushite is anisotropic, with the largest expansion along the b axis due principally to the effect of the O(1)···D(4) and O(3)···D(2) hydrogen bonds. Expansion along the c axis, influenced by the Ow1···D(5) interwater hydrogen bond, is also large. The high temperature limits for the expansion coefficients for the unit-cell edges a, b and c are 9.7(5) × 10-6, 3.82(9) × 10-5 and 5.54(5) × 10-5 K-1, respectively, and for the cell volume it is 9.7(1) × 10-5 K-1. The β angle displays oscillatory variation, and empirical data analysis results in αβ = 1.28(3) × 10-6sin(0.0105 T) K-1, within this temperature range. The evolution of the thermal expansion tensor of brushite has been calculated between 50 ≤T≤ 400 K. At 300 K the magnitudes of the principal axes are α11 = 50(6) × 10-6 K-1, α22 = 26.7(7) × 10-6 K-1 and α33 = 7.0(5) × 10-6 K-1. The intermediate axis, α22, is parallel to b, and using IRE convention for the tensor orthonormal basis, the axes α11 and α33 have directions equal to (-0.228, 0, -0.974) and (-0.974, 0, 0.228) respectively. Under the conditions of these experiments, the onset of dehydration occurred at temperatures above 400 K. Bond valence analysis combined with assessments of the thermal evolution of the bonding within brushite suggests that dehydration is precipitated through instabilities in the chemical environment of the second water molecule.

  16. The role of brushite and octacalcium phosphate in apatite formation.

    Science.gov (United States)

    Johnsson, M S; Nancollas, G H

    1992-01-01

    Studies of apatite mineral formation are complicated by the possibility of forming several calcium phosphate phases. The least soluble, hydroxyapatite (HAP), is preferentially formed under neutral or basic conditions. In more acidic solutions phases such as dicalcium phosphate dihydrate (Brushite, DCPD) and octacalcium phosphate (OCP) are often found. Even under ideal HAP precipitation conditions the precipitates are generally nonstoichiometric, suggesting the formation of calcium-deficient apatites. Both DCPD and OCP have been implicated as possible precursors to the formation of apatite. This may occur by the initial precipitation of DCPD and/or OCP followed by transformation to a more apatitic phase. Although DCPD and OCP are often detected during in vitro crystallization, in vivo studies of bone formation rarely show the presence of these acidic calcium phosphate phases. In the latter case the situation is more complicated, since a large number of ions and molecules are present that can be incorporated into the crystal lattice or adsorbed at the crystallite surfaces. In biological apatite, DCPD and OCP are usually detected only during pathological calcification where the pH is often relatively low. In normal in vivo calcifications these phases have not been found, suggesting the involvement of other precursors or the formation of an initial amorphous calcium phosphate phase (ACP) followed by transformation to apatite.

  17. Dual roles of brushite crystals in calcium oxalate crystallization provide physicochemical mechanisms underlying renal stone formation.

    Science.gov (United States)

    Tang, R; Nancollas, G H; Giocondi, J L; Hoyer, J R; Orme, C A

    2006-07-01

    Calcium oxalate monohydrate (COM) crystals are the major mineral component of most kidney stones, and thus have an important role in chronic human disease. However, the physicochemical mechanisms leading to calcium oxalate (CaOx) stone disease are only partially defined. As spontaneous precipitation of CaOx is rare under renal conditions, an alternative pathway for CaOx crystallization seems necessary to resolve this central issue. We performed kinetic studies using the dual constant composition method to simultaneously analyze the crystallization of COM and brushite, the form of calcium phosphate that is most readily formed in the typical slightly acidic urinary milieu. These studies were supported by parallel analysis by scanning electron and atomic force microscopy. In these studies, mineralization of a thermodynamically stable phase (COM) was induced by the presence of brushite, a more readily precipitated inorganic phase. Furthermore, once formed, the COM crystals grew at the expense of brushite crystals causing the dissolution of the brushite crystals. These studies show that brushite may play crucial roles in the formation of COM crystals. The definition of these two roles for brushite thereby provides physicochemical explanations for the initiation of COM crystallization and also for the relative paucity of calcium phosphate detected in the majority of CaOx renal stones.

  18. Crystallo-chemical analyses of calcium phosphates

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    Sakae, Toshiro; Hayakawa, Tohru; Maruyama, Fumiaki; Nemoto, Kimiya; Kozawa, Yukishige [Nihon Univ., Matsudo, Chiba (Japan). School of Dentistry

    1997-12-01

    Several analytical techniques, methodology and their practical data processing were briefly described to investigate the crystallographic properties of calcium phosphates which are encountered in the field of dental sciences. The applied analytical techniques were X-ray fluorescence spectrometry (XFS), energy dispersive spectrometry (EDS), Fourier transform infrared spectrometry (FT-IR) and X-ray diffraction (XRD). The used materials were tetracalcium phosphate, hydroxyapatite, fluorapatite, {alpha}-tricalcium phosphate, {beta}-tricalcium phosphate, octacalcium phosphate, monetite, brushite and monocalcium phosphate monohydrate. (author)

  19. Potential etiologic role of brushite in the formation of calcium (renal) stones

    Science.gov (United States)

    Pak, Charles Y. C.

    1981-05-01

    Brushite may play an important regulatory role in the formation of calcium -containing renal stones. The urinary environment from patients with hypercalciuric nephrolithiasis is typically supersaturated and shows an increased propensity for the spontaneous nucleation of brushite. Brushite has been identified in "stone-forming" urine and in stones. This crystalline phase may undergo phase transformation to hydroxyapatite or cause heterogeneous nucleation or epitaxial growth of calcium oxalate. Thus, brushite may also participate in the formation of stones of hydroxypatite or calcium oxalate.

  20. Beta-tricalcium phosphate release from brushite cement surface.

    Science.gov (United States)

    Alkhraisat, M Hamdan; Mariño, F Tamimi; Retama, J Rubio; Jerez, L Blanco; López-Cabarcos, E

    2008-03-01

    Different in vivo studies demonstrated that brushite cements are biocompatible, bioresorbable, and osteoconductive. However, the decay of brushite cements has been scarcely studied even though it may be of great concern for clinical applications in highly blood-perfused regions. This work was elaborated to elucidate factors that determine brushite cement surface disintegration. For that, brushite cements were modified using in their preparation different aqueous solutions of phosphoric, glycolic, tartaric, and citric acids in concentrations that were reported to improve the cement properties. Two-viscosity enhancing polysaccharides, chondroitin-4 sulfate and hyaluronic acid, were also assayed. Thereafter, pre- and set cement samples were immersed in distilled water for 24 h. The cement-solid weight loss, microstructure, liquid phase viscosity, mean size of the released particles, and zeta potential were analyzed using X-ray diffraction, FTIR spectroscopy, light scattering, scanning electron microscopy and optical microscopy. It was found that the particles released from the cement surface were beta-TCP, and their amount depends on the carboxylic acid used in the preparation of the cement. The addition of hyaluronic acid and chondroitin-4 sulfate decreased the amount of released particles from the surface of the set brushite cement made with citric acid. Furthermore, the hyaluronic acid increased significantly the viscosity of the citric acid solution and the cement paste prepared with this liquid phase showed a pronounced step down in particle release. In this study, we showed that the water solubility of calcium carboxylate and the viscosity of mixing liquid may dictate the superficial disintegration of brushite cements.

  1. In vitro precipitation of calcium phosphate under intracellular conditions: formation of brushite from an amorphous precursor in the absence of ATP.

    Science.gov (United States)

    Wuthier, R E; Rice, G S; Wallace, J E; Weaver, R L; LeGeros, R Z; Eanes, E D

    1985-07-01

    Release of mitochondrial calcium has been shown to occur concomitant with mineral ion loading of matrix vesicles at the onset of mineralization in epiphyseal growth plate cartilage. Matrix vesicles contain amorphous calcium phosphate (ACP), a mineral form that usually results from rapid precipitation at high initial levels of Ca2+ and/or inorganic P (Pi). Since the cytosol of growth plate chondrocytes has been found to contain high levels of Pi, rapid release of mitochondrial Ca2+ into the cytosol may cause local precipitation of calcium phosphate and thus be coupled with matrix vesicle formation. Studies were carried out to determine the kinetics and nature of mineral formation that occur when small amounts of Ca2+ are added under various conditions to a Pi buffer composed of electrolytes matched in concentrations and pH to that of the cytosol of epiphyseal chondrocytes. Depending on the manner in which Ca2+ was added, ACP, dicalcium phosphate dihydrate (DCPD), or apatite (HA) first formed. In the presence of ATP, ACP was the only solid phase detected, being stable for at least 24 h. However, in its absence, ACP rapidly transformed into DCPD. Increasing the pH of the reaction buffer from 6.9 to 7.5 increased the amount of ACP initially formed, but DCPD was consistently found upon ACP transformation. Yet at pH 8.0, ACP persisted for at least 24 h. The amount of precipitate formed was proportional to the level of added Ca2+; precipitates formed when as little as 1.0 mmole was added per liter of buffer. Our findings support the possibility that rapid release of mitochondrial Ca2+ may cause localized intracellular precipitation of ACP. Since nascent ACP is known to stimulate membrane fusion and blebbing of vesicles, these findings may explain the presence of ACP in matrix vesicles. The rapid conversion of ACP to DCPD in the absence of ATP under these conditions may also explain the reported occurrence of DCPD in samples of early mineralizing tissue.

  2. Crystallization of brushite from EDTA-chelated calcium in agar gels

    Science.gov (United States)

    Plovnick, Ross H.

    1991-10-01

    Brushite (dicalcium phosphate dihydrate, CaHPO 4·2H 2O, DCPD) has been crystallized from ethylenediaminetetraacetic acid (EDTA)-chelated calcium in agar gels at initial pH 4.5-6.4 and Ca/P molar ratio above about 0.8. White, spherular crystalline DCPD aggregates up to 1 mm in diameter grew in 8-10 weeks. Liesegang ring were occassionally observed at initial gel pH 5 and Ca/P molar ratio near 1. Crystals were characterized by X-ray diffraction analysis, scanning electron microscopy, and infrared absorption spectroscopy. Brushite crystals were also grown in agar gels with either unchelated Ca initially present in the gels and EDTA in overlying solutions, or EDTA initially present in the gels and unchelated Ca in overlying solutions. These crystals grew as 2-3 mm aggregates mainly within 1-3 cm of the gel-solution interface.

  3. Molecular mechanisms of crystallization impacting calcium phosphate cements

    OpenAIRE

    2010-01-01

    The biomineral calcium hydrogen phosphate dihydrate (CaHPO4·2H2O), known as brushite, is a malleable material that both grows and dissolves faster than most other calcium minerals, including other calcium phosphate phases, calcium carbonates and calcium oxalates. Within the body, this ready formation and dissolution can play a role in certain diseases, such as kidney stone and plaque formation. However, these same properties, along with brushite’s excellent biocompatibility, can be used to gr...

  4. Brushite Stone Disease as a Consequence of Lithotripsy?

    OpenAIRE

    2010-01-01

    The incidence of calcium phosphate (CaP) stone disease has increased over the last three decades; specifically, brushite stones are diagnosed and treated more frequently than in previous years. Brushite is a unique form of CaP, which in certain patients can form into large symptomatic stones. Treatment of brushite stones can be difficult since the stones are resistant to shock wave and ultrasonic lithotripsy, and often require ballistic fragmentation. Patients suffering from brushite stone di...

  5. Phase transformations, microstructure formation and in vitro osteoblast response in calcium silicate/brushite cement composites.

    Science.gov (United States)

    Sopcak, T; Medvecky, L; Giretova, M; Kovalcikova, A; Stulajterova, R; Durisin, J

    2016-08-10

    Self-setting simple calcium silicate/brushite (B) biocements with various Ca/P ratios were prepared by mutual mixing of both monocalcium silicate hydrate (CSH) or β-wollastonite (woll) powders with B and the addition of 2 wt% NaH2PO4 solution as a hardening liquid. The phase composition of the final composites and the texture of the surface calcium phosphate/silica layer were controlled by the starting Ca/P ratio in composites and the pH during setting. It was verified that the presence of continuous bone-like calcium phosphate coating on the surface of the samples was not essential for in vitro osteoblast proliferation. The nanocrystalline calcium deficient hydroxyapatite and amorphous silica were found as the main setting products in composite mixtures with a Ca/P ratio close to the region of the formation of deficient hydroxyapatite-like calcium phosphates. No CSH phase with a lower Ca/Si ratio was identified after transformation. The results confirmed a small effect of the monocalcium silicate addition on the compressive strength (CS) of cements up to 30 wt% (around 20-25 MPa) and a significant rise of the value in 50 woll/B cement (65 MPa). The final setting times of the cement composites varied between 5 and 43 min depending on the P/L ratio and the type of monocalcium silicate phase in the cement mixture. 10CSH/B and 50 woll/B cements with different textures but free of both the needle-like and perpendicularly-oriented hydroxyapatite particles on the surface of the samples had low cytotoxicity.

  6. Precipitation of calcium phosphate at 40° C from neutral solution

    Science.gov (United States)

    Lundager Madsen, Hans E.; Christensson, Finn

    1991-12-01

    Calcium phosphate formation was studied in the pH range 5brushite (CaHPO 4·2H 2O) is the role product, and octacalcium phosphate predominates at low concentrations. ACP is subsequently transformed into brushite or apatite (Ca 5OH(PO 4) 3), the latter always crytocrystalline, but brushite crystals often redissolve and leave apatite as the end product. The formation and evolution of precipitates are chiefly governed by solubilities of the different crystalline phases; for apatite, the excess solubility of small crystals as determined by the Gibbs-Kelvin equation plays an important role.

  7. The effect of autoclaving on the physical and biological properties of dicalcium phosphate dihydrate bioceramics: brushite vs. monetite.

    Science.gov (United States)

    Tamimi, Faleh; Le Nihouannen, Damien; Eimar, Hazem; Sheikh, Zeeshan; Komarova, Svetlana; Barralet, Jake

    2012-08-01

    Dicalcium phosphate dihydrate (brushite) is an osteoconductive biomaterial with great potential as a bioresorbable cement for bone regeneration. Preset brushite cement can be dehydrated into dicalcium phosphate anhydrous (monetite) bioceramics by autoclaving. This heat treatment results in changes in the physical characteristics of the material, improving in vivo bioresorption. This property is a great advantage in bone regeneration; however, it is not known how autoclaving brushite preset cement might improve its capacity to regenerate bone. This study was designed to compare brushite bioceramics with monetite bioceramics in terms of physical characteristics in vitro, and in vivo performance upon bone implantation. In this study we observed that monetite bioceramics prepared by autoclaving preset brushite cements had higher porosity, interconnected porosity and specific surface area than their brushite precursors. In vitro cell culture experiments revealed that bone marrow cells expressed higher levels of osteogenic genes Runx2, Opn, and Alp when the cells were cultured on monetite ceramics rather than on brushite ones. In vivo experiments revealed that monetite bioceramics resorbed faster than brushite ones and were more infiltrated with newly formed bone. In summary, autoclaving preset brushite cements results in a material with improved properties for bone regeneration procedures.

  8. Molecular mechanisms of crystallization impacting calcium phosphate cements.

    Science.gov (United States)

    Giocondi, Jennifer L; El-Dasher, Bassem S; Nancollas, George H; Orme, Christine A

    2010-04-28

    The biomineral calcium hydrogen phosphate dihydrate (CaHPO(4).2H(2)O), known as brushite, is a malleable material that both grows and dissolves faster than most other calcium minerals, including other calcium phosphate phases, calcium carbonates and calcium oxalates. Within the body, this ready formation and dissolution can play a role in certain diseases, such as kidney stone and plaque formation. However, these same properties, along with brushite's excellent biocompatibility, can be used to great benefit in making resorbable biomedical cements. To optimize cements, additives are commonly used to control crystallization kinetics and phase transformation. This paper describes the use of in situ scanning probe microscopy to investigate the role of several solution parameters and additives in brushite atomic step motion. Surprisingly, this work demonstrates that the activation barrier for phosphate (rather than calcium) incorporation limits growth kinetics and that additives such as magnesium, citrate and bisphosphonates each influence step motion in distinctly different ways. Our findings provide details of how, and where, molecules inhibit or accelerate kinetics. These insights have the potential to aid in designing molecules to target specific steps and to guide synergistic combinations of additives.

  9. Solid state NMR study calcium phosphate ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Miquel, J.L.; Facchini, L.; Legrand, A.P. (Laboratoire de Physique Quantique, Paris (France). CNRS, URA421, ESPCI); Rey, C. (CNRS, Toulouse (France). ENSC. Laboratoire de Physico-chimie des Solides); Lemaitre, J. (EPF Lausanne (France). Laboratoire de Technologie des Poudres)

    1990-04-01

    High-resolution {sup 31}P and {sup 1}H NMR spectra at 40 and 121 MHz {sup 31}P and 300 MHz {sup 1}H of synthetic and biological samples of calcium phosphates have been obtained by magic angle spinning (MAS) at spinning speeds up to 6.5 kHz, and high power proton decoupling. The samples include crystalline hydroxyapatite, a deficient hydroxyapatite characterized by a Ca/P atomic ratio of 1.5, a poorly crystallized hydroxyapatite, monetite, brushite, octacalcium phosphate, {beta}-tricalcium phosphate and rabbit femoral bone. The interactions between nuclei in unlike structures and the mobility of acid protons are discussed. (author). 11 refs.; 2 figs.; 1 tab.

  10. Precipitation of calcium phosphate from moderately acid solution

    Science.gov (United States)

    Lundager Madsen, H. E.; Thorvardarson, G.

    1984-04-01

    The precipitation of calcium phosphate upon mixing of equimolar amounts of calcium nitrate and ammonium phosphate has been studied in the temperature range 40-60°C and pH 3.5-6.5. At the lowertemperatures, brushite, CaHPO 4, 2 H 2O, is the major crystalline product. Monetite, CaHPO 4, is formed at the higher temperatures and above a certain critical supersaturation, and OCP, Ca 4H(PO 4) 3.2.5H 2O, in the higher pH range. A metastable, amorphous tricalcium phosphate, Ca 3(PO 4) 2. xH2O, is formed initially if a(Ca 2+) 3a(PO 3-4) 2 exceeds a certain value, which decreases rapidly as temperature increases. The range in which brushite is found as the only crystalline phase narrows with increasing temperature. The results are explained in terms of heterogeneous nucleation for brushite and homogeneous nucleation for monetite.

  11. Molecular mechanisms of crystallization impacting calcium phosphate cements

    Science.gov (United States)

    Giocondi, Jennifer L.; El-Dasher, Bassem S.; Nancollas, George H.; Orme, Christine A.

    2010-01-01

    The biomineral calcium hydrogen phosphate dihydrate (CaHPO4·2H2O), known as brushite, is a malleable material that both grows and dissolves faster than most other calcium minerals, including other calcium phosphate phases, calcium carbonates and calcium oxalates. Within the body, this ready formation and dissolution can play a role in certain diseases, such as kidney stone and plaque formation. However, these same properties, along with brushite’s excellent biocompatibility, can be used to great benefit in making resorbable biomedical cements. To optimize cements, additives are commonly used to control crystallization kinetics and phase transformation. This paper describes the use of in situ scanning probe microscopy to investigate the role of several solution parameters and additives in brushite atomic step motion. Surprisingly, this work demonstrates that the activation barrier for phosphate (rather than calcium) incorporation limits growth kinetics and that additives such as magnesium, citrate and bisphosphonates each influence step motion in distinctly different ways. Our findings provide details of how, and where, molecules inhibit or accelerate kinetics. These insights have the potential to aid in designing molecules to target specific steps and to guide synergistic combinations of additives. PMID:20308110

  12. Obtaining Ca(H2PO4)(2)·H2O, monocalcium phosphate monohydrate, via monetite from brushite by using sonication.

    Science.gov (United States)

    Sánchez-Enríquez, J; Reyes-Gasga, J

    2013-05-01

    Brushite was synthesized by precipitation of calcium chloride (CaCl(2)) and sodium phosphate monobasic (Na(2)HPO(4)) dried in vacuum and monetite was obtained from this brushite by sonication with a frequency of 90kHz at 500W for 90min. Monetite itself was also transformed in Ca(H(2)PO(4))(2)·H(2)O, monocalcium phosphate monohydrate (MCPM), by sonication with a frequency of 90kHz at 500W for 60min followed by lyophilization. The MCPM was sonicated and lyophilized by three times more until reach over 240min, but any other phase transformation was observed. All these phase transformations were analyzed by X-ray diffraction (XRD) and infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated a grain size of about 200nm in all the samples. The morphology observed was a corn-flake-like grain for brushite, a pseudo-needle-like grains for monetite, and lamellar-like grains for MCPM.

  13. Incorporation of a controlled-release glass into a calcium phosphate cement.

    Science.gov (United States)

    Khairoun, I; Boltong, M G; Gil, F J; Driessens, F C; Planell, J A; Seijas, M M; Martínez, S

    1999-04-01

    A so-called controlled-release glass was synthesized occurring in the system CaO-Na2O-P2O5. A certain sieve fraction of this glass was incorporated in a calcium phosphate cement, of which the powder contained alpha-tricalcium phosphate (alpha-TCP), dicalcium phosphate (DCP) and precipitated hydroxyapatite (HA). The glass appeared to retard the cement setting slightly and it reduced considerably the compressive strength after aging in aqueous solutions which were continuously refreshed. Scanning electron microscope (SEM) pictures and X-ray diffraction (XRD) patterns of the samples after 5 weeks of aging showed that the glass was not dissolved but that large brushite crystals were formed. Thereby, aging in CaCl2 solutions resulted in more brushite formation than aging in NaCl solutions. The brushite crystals did not reinforce the cement. Neither was the aged glass-containing cement weaker than it was before the brushite formation right after complete setting. In conclusion, the incorporation of controlled-release glasses into a calcium phosphate cement and subsequent aging in aqueous solutions did not result in the formation of macropores in the cement structure, but that of brushite crystals. This incorporation reduced the compressive strength of the cement considerably.

  14. Porosity prediction of calcium phosphate cements based on chemical composition.

    Science.gov (United States)

    Öhman, Caroline; Unosson, Johanna; Carlsson, Elin; Ginebra, Maria Pau; Persson, Cecilia; Engqvist, Håkan

    2015-07-01

    The porosity of calcium phosphate cements has an impact on several important parameters, such as strength, resorbability and bioactivity. A model to predict the porosity for biomedical cements would hence be a useful tool. At the moment such a model only exists for Portland cements. The aim of this study was to develop and validate a first porosity prediction model for calcium phosphate cements. On the basis of chemical reaction, molar weight and density of components, a volume-based model was developed and validated using calcium phosphate cement as model material. 60 mol% β-tricalcium phosphate and 40 mol% monocalcium phosphate monohydrate were mixed with deionized water, at different liquid-to-powder ratios. Samples were set for 24 h at 37°C and 100% relative humidity. Thereafter, samples were dried either under vacuum at room temperature for 24 h or in air at 37 °C for 7 days. Porosity and phase composition were determined. It was found that the two drying protocols led to the formation of brushite and monetite, respectively. The model was found to predict well the experimental values and also data reported in the literature for apatite cements, as deduced from the small absolute average residual errors (brushite, monetite and apatite cements. The model gives a good estimate of the final porosity and has the potential to be used as a porosity prediction tool in the biomedical cement field.

  15. Influence of foreign metal ions on crystal growth and morphology of brushite (CaHPO 4, 2H 2O) and its transformation to octacalcium phosphate and apatite

    Science.gov (United States)

    Lundager Madsen, Hans E.

    2008-05-01

    Brushite, forming tabular crystals, has been precipitated at 25 °C in the presence of each of 14 different di- and trivalent metal ions. The influence of these ions at micromolar concentrations on the solvent-mediated phase transformation of brushite to more basic calcium phosphates has been studied as well. The effect of additives on brushite crystallization was pH-dependent, which could be related to the presence or absence of amorphous precipitate. In the latter case the course of the crystallization process could be followed by recording pH as function of time. For half of the additives kinetic analysis was possible and showed that the crystal growth mechanism is surface nucleation. Edge free energy is lowered in the presence of an additive. Zn favoured aggregates, and the transition metals with the exceptions of Mn(II), Co(II) and Cu(II) favoured irregular growth. Zn inhibited lateral growth, as did Cd and Cr(III) at low and Cu(II) at high pH. Most of the ions have a marked effect on the transformation to octacalcium phosphate (OCP) and hydroxyapatite (HAP) as well. In both cases Cu(II) and Zn are strong inhibitors, whereas Pb(II) is a moderate promotor. Fe in both oxidation states, Co(II), Mn(II) and Sr are intermediate in effect on phase transformation. Inhibition may be caused by adsorbed foreign ions impeding growth of nuclei or by poisoning of the substrate for heterogeneous nucleation, i.e. brushite crystals. Promotion is explained by the formation of nuclei with suitable crystal structure, e.g. apatite/pyromorphite (Ca,Pb) 5OH(PO 4) 3 in the case of Pb.

  16. Cellular investigations on electrochemically deposited calcium phosphate composites.

    Science.gov (United States)

    Becker, Petra; Neumann, Hans-Georg; Nebe, Barbara; Lüthen, Frank; Rychly, Joachim

    2004-04-01

    Electrochemically deposited calcium phosphate (CaP) coatings are fast resorbable and existent only during the first period of osseointegration. In the present study, composite coatings with varying solubility (hydroxyapatite (HA), brushite with less HA and monetite (M) with less HA) were prepared and the influence of the degradation and the reprecipitation of CaP on osteoblastic cells were investigated. On the brushite composite coating a new precipitated, finely structured CaP phase was observed during immersion in cell culture medium with or without osteoblastic cells. The surface morphology of monetite and HA coatings were entirely unmodified under the same conditions. So it could be assumed that electrochemically deposited brushite with less HA acts as a precursor for new precipitated CaP. On this surface osteoblastic cells revealed a well-spread morphology with pronounced actin cytoskeleton and demonstrated good proliferation behaviour. Thus we suggest that brushite seems to be especially suitable for coating of implants as a matrix for nucleation and growth of new bone.

  17. Evaluation of a porosity measurement method for wet calcium phosphate cements.

    Science.gov (United States)

    Ajaxon, Ingrid; Maazouz, Yassine; Ginebra, Maria-Pau; Öhman, Caroline; Persson, Cecilia

    2015-11-01

    The porosity of a calcium phosphate cement is a key parameter as it affects several important properties of the cement. However, a successful, non-destructive porosity measurement method that does not include drying has not yet been reported for calcium phosphate cements. The aim of this study was to evaluate isopropanol solvent exchange as such a method. Two different types of calcium phosphate cements were used, one basic (hydroxyapatite) and one acidic (brushite). The cements were allowed to set in an aqueous environment and then immersed in isopropanol and stored under three different conditions: at room temperature, at room temperature under vacuum (300 mbar) or at 37℃. The specimen mass was monitored regularly. Solvent exchange took much longer time to reach steady state in hydroxyapatite cements compared to brushite cements, 350 and 18 h, respectively. Furthermore, the immersion affected the quasi-static compressive strength of the hydroxyapatite cements. However, the strength and phase composition of the brushite cements were not affected by isopropanol immersion, suggesting that isopropanol solvent exchange can be used for brushite calcium phosphate cements. The main advantages with this method are that it is non-destructive, fast, easy and the porosity can be evaluated while the cements remain wet, allowing for further analysis on the same specimen.

  18. Brushite stone disease as a consequence of lithotripsy?

    Science.gov (United States)

    Krambeck, Amy E; Handa, Shelly E; Evan, Andrew P; Lingeman, James E

    2010-08-01

    The incidence of calcium phosphate (CaP) stone disease has increased over the last three decades; specifically, brushite stones have been diagnosed and treated more frequently than in previous years. Brushite is a unique form of CaP, which in certain patients can form into large symptomatic stones. Treatment of brushite stones can be difficult since the stones are resistant to shock wave and ultrasonic lithotripsy, and often require ballistic fragmentation. Patients suffering from brushite stone disease are less likely to be rendered stone free after surgical intervention and often experience stone recurrence despite maximal medical intervention. Studies have demonstrated an association between brushite stone disease and shock wave lithotripsy (SWL) treatment. Some have theorized that many brushite stone formers started as routine calcium oxalate (CaOx) stone formers who sustained an injury to the nephron (such as SWL). The injury to the nephron leads to failure of urine acidification and eventual brushite stone formation. We explore the association between brushite stone disease and iatrogenic transformation of CaOx stone disease to brushite by reviewing the current literature.

  19. Calcium Phosphate Biomaterials: An Update

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Current calcium phosphate (CaP) biomaterials for bone repair, substitution, augmentation and regeneration include hydroxyapatite ( HA ) from synthetic or biologic origin, beta-tricalcium phosphate ( β-TCP ) , biphasic calcium phosphate (BCP), and are available as granules, porous blocks, components of composites (CaP/polymer) cements, and as coatings on orthopedic and dental implants. Experimental calcium phosphate biomaterials include CO3- and F-substituted apatites, Mg-and Zn-substituted β-TCP, calcium phosphate glasses. This paper is a brief review of the different types of CaP biomaterials and their properties such as bioactivity, osteoconductivity, osteoinductivity.

  20. Contrasting histopathology and crystal deposits in kidneys of idiopathic stone formers who produce hydroxy apatite, brushite, or calcium oxalate stones.

    Science.gov (United States)

    Evan, Andrew P; Lingeman, James E; Worcester, Elaine M; Sommer, Andre J; Phillips, Carrie L; Williams, James C; Coe, Fredric L

    2014-04-01

    Our previous work has shown that stone formers who form calcium phosphate (CaP) stones that contain any brushite (BRSF) have a distinctive renal histopathology and surgical anatomy when compared with idiopathic calcium oxalate stone formers (ICSF). Here we report on another group of idiopathic CaP stone formers, those forming stone containing primarily hydroxyapatite, in order to clarify in what ways their pathology differs from BRSF and ICSF. Eleven hydroxyapatite stone formers (HASF) (2 males, 9 females) were studied using intra-operative digital photography and biopsy of papillary and cortical regions to measure tissue changes associated with stone formation. Our main finding is that HASF and BRSF differ significantly from each other and that both differ greatly from ICSF. Both BRSF and ICSF patients have significant levels of Randall's plaque compared with HASF. Intra-tubular deposit number is greater in HASF than BRSF and nonexistent in ICSF while deposit size is smaller in HASF than BRSF. Cortical pathology is distinctly greater in BRSF than HASF. Four attached stones were observed in HASF, three in 25 BRSF and 5-10 per ICSF patient. HASF and BRSF differ clinically in that both have higher average urine pH, supersaturation of CaP, and calcium excretion than ICSF. Our work suggests that HASF and BRSF are two distinct and separate diseases and both differ greatly from ICSF.

  1. Optimizing Calcium Phosphates by the Control of pH and Temperature via Wet Precipitation.

    Science.gov (United States)

    Kim, YoungJae; Lee, Seon Yong; Roh, Yul; Lee, Jinhyeok; Kim, Juyeun; Lee, Yongwoo; Bang, Junseok; Lee, Young Jae

    2015-12-01

    A series of calcium phosphates synthesized through a wet precipitation route of hydroxylapatite (HAP) was investigated over a wide range of temperature and pH (25-80 degrees C, and pH 6.5-10.0) using a combination of microscopic and spectroscopic analyses. XRD and FTIR show that monetite and brushite are formed as a single phase at non-ideal conditions of HAP, respectively. From TGA results, it is found that brushite is converted to monetite at a range 175-200 degrees C when heated at the heating rate, 10 degrees C/min. This phase transformation is also observed when brushite is aged at pH 8.5 and 60 degrees C for 24 hr in solution. Morphology of brushite is sensitive to pH variation. At pH 6.5, tabular and platy crystals of brushite are observed whereas needle-like ones are predominant at pH 8.5. For HAP formed at pH 10.0, their shapes tend toward needle-like particles as temperature increases. HAP particles at pH 8.5 are very similar in morphology to HAP at pH 10.0, but their lengths are two or three times as great as those at pH 10.0. These observations demonstrate that desired phase and properties of calcium phosphates can be controlled by pH, temperature, and aging time through a wet precipitation method.

  2. Biomimetic Nanocomposites of Calcium Phosphate and Self-Assembling Triblock and Pentablock Copolymers

    Energy Technology Data Exchange (ETDEWEB)

    Enlow, Drew Lenzen [Iowa State Univ., Ames, IA (United States)

    2006-01-01

    In an effort to mimic the growth of natural bone, self-assembling, micelle and gel-forming copolymers were used as a template for calcium phosphate precipitation. Because of the cationic characteristics imparted by PDEAEM end group additions to commercially available Pluronic{reg_sign} Fl27, a direct ionic attraction mechanism was utilized and a polymer-brushite nanocomposite spheres were produced. Brushite coated spherical micelles with diameters of ~40 nm, and agglomerates of these particles (on the order of 0.5 μm) were obtained. Thickness and durability of the calcium phosphate coating, and the extent of agglomeration were studied. The coating has been shown to be robust enough to retain its integrity even below polymer critical micelle concentration and/or temperature. Calcium phosphate-polymer gel nanocomposites were also prepared. Gel samples appeared as a single phase network of agglomerated spherical micelles, and had a final calcium phosphate concentration of up to 15 wt%. Analysis with x-ray diffraction and NMR indicated a disordered brushite phase with the phosphate groups linking inorganic phase to the polymer.

  3. Morphology control of brushite prepared by aqueous solution synthesis

    OpenAIRE

    2014-01-01

    Dicalcium phosphate dihydrate (DCPD, CaHPO4·2H2O), also known as brushite, is one of the important bioceramics due to not only diseases factors such as kidney stone and plaque formation but also purpose as fluoride insolubilization material. It is used medicinally to supply calcium, and is of interest for its unique properties in biological and pathological mineralization. It is important to control the crystal morphology of brushite since its chemical reactivity depends strongly on its surfa...

  4. The influence of magnetism on precipitation of calcium phosphate

    Science.gov (United States)

    Skytte Sørensen, Jens; Lundager Madsen, Hans E.

    2000-06-01

    The precipitation of calcium phosphate upon rapid mixing of solutions of CaCl 2 and KH 2PO 4-K 2HPO 4 was followed by pH and other quantitative measurements and the examination of the precipitate in the polarizing microscope. The experiments were carried out at 25°C in the presence and absence of a static magnetic field of 0.27 T. It was found that the magnetic field increased dissolution of metastable precursor phases and increased nucleation of more stable phases. This was a general tendency for the transformation sequence: ACP→ brushite →OCP→HAP at initial pH≈6.5 and total concentrations CCa= CP=25, 50 or 100 mM. Crystallization upon slow diffusion of ions from a solution of CaCl 2 into silica hydrogel containing dissolved KH 2PO 4-K 2HPO 4 was followed by recording the number and positions of appearing brushite crystals and Liesegang rings. The experiment was performed in the presence and absence of magnetic fields in the range 0.08-0.3 T and the following conditions: room temperature, initial pH of the gel between 5.5 and 6.8, and CCa= CP=50 mM. Magnetism increased nucleation of brushite in the experiments at low initial pH. The dependence on field strength was not significant, and no effect was found in experiments with high initial pH.

  5. In-situ mineralization of chitosan/calcium phosphate composite and the effect of solvent on the structure

    Science.gov (United States)

    He, Ling-Hao; Yao, Lu; Xue, Rui; Sun, Jing; Song, Rui

    2011-09-01

    Solvent played an important role in the formation of calcium phosphate phase of the chitosan/calcium phosphate composites. In this investigation, ethanolacetic acid mixtures were employed as solvents, and various calcium phosphate phases, such as brushite, amorphous calcium phosphate, and hydroxyapatite, were introduced into the chitosan/calcium phosphate composites by using in-situ preparation process. The results showed that the structures of composite were influenced remarkably by the morphology and the distribution of calcium phosphate phase. In addition, the bioactivity of composites was governed mainly by the characters of calcium phosphate phases in composites, since calcium phosphate phases could induce the growth of hydroxyapatite coating on the surfaces of composites. On the surface of chitosan/brushite composite, the formed hydroxyapatite coating consisted of oriented plate crystallites, which selfassembled into spherical-like crystals. When other calcium phosphate phase was introduced into composites, the polymorphs of hydroxyapatite layer would change greatly. The oriented plate crystallites became bigger, and meanwhile, the self-assembled aggregates became less and smaller. In addition, with the shift of the prior nucleating point, the growth orientation of plate crystallites was transformed.

  6. Transformation of modified brushite to hydroxyapatite in aqueous solution: effects of potassium substitution.

    Science.gov (United States)

    Kumar, M; Xie, J; Chittur, K; Riley, C

    1999-08-01

    Brushite (dicalcium phosphate dihydrate, DCPD, CaHPO4 x 2H2O) was deposited electrolytically from calcium dihydrogen phosphate solution with and without potassium chloride (KCl) as a supporting electrolyte. The kinetics of brushite transformation to hydroxyapatite (HA, Ca5(PO4)3OH) in the presence of calcium and protein free, aqueous body fluid (Hank's balanced salt solution, HBSS) was investigated. We present evidence that the deposition of brushite in a KCl-supported electrochemical bath yields a modified brushite where some of the calcium is substituted by potassium. Transformation of both normal (i.e. potassium free) and modified brushite to hydroxyapatite upon exposure to calcium and protein-free aqueous fluid (HBSS) was followed by reflectance Fourier Transform Infrared (FTIR) spectroscopy and X-ray diffraction (XRD) techniques. Changes in the morphology of the coatings were studied using scanning electron microscopy (SEM). Results indicate that modified brushite undergoes faster transformation to hydroxyapatite in HBSS in comparison to normal brushite. Our results show that the presence of potassium ions in the brushite not only favors the formation of different intermediate phases but also alters transformation rates to HA.

  7. The gypsum-brushite system: crystallization from solutions poisoned by phosphate ions

    Science.gov (United States)

    Rinaudo, C.; Lanfranco, A. M.; Boistelle, R.

    1996-01-01

    Gypsum and a non-stoichiometric calcium phosphate sulphate hydrate (CPSH) were grown from solutions poisoned by phosphate ions. The pH ranged from 4.7 to 5.6 and the sulphate over phosphate ratios from 1.5 to 9. In some cases, when the phosphate concentration was high (30%-40%) CPSH was stable. When the phosphate concentration was lower (10%-20%), CPSH formed as first phase in association with gypsum, but dissolved as soon as gypsum crystallized and grew at its expense. In that case, gypsum contained up to 10% phosphate. On the other hand, when gypsum crystallized alone, as first phase, it did not contain detectable amounts of phosphate.

  8. The initial phases of calcium and magnesium phosphates precipitated from solutions of high to medium concentrations

    Science.gov (United States)

    Abbona, F.; Madsen, H. E. Lundager; Boistelle, R.

    1986-04-01

    The precipitation of calcium and magnesium phosphates is performed at 25°C by mixing solutions of ammonium phosphate and solutions of calcium and magnesium chlorides under the condition [ P] = [ Ca] + [ Mg] in large pH intervals. Before any nucleation the phosphate concentration ranges from 0.50M to 0.01M. The phases first precipitated are CaHPO 4·2H 2O (brushite), CaHPO 4 (monetite), Ca 3(PO 4) 2· xH 2O (amorphous calcium phosphate), MgNH 4PO 4·6H 2O (struvite), and MgHPO 4·3H 2O (newberyite). The precipitation fields of each phase are determined and discussed as a function of pH, composition and supersaturation. The solutions are even supersaturated with respect to several other calcium phosphates but they never occur first even if their supersaturation is the highest.

  9. Experimental study of brushite precipitation

    Science.gov (United States)

    Arifuzzaman, S. M.; Rohani, S.

    2004-07-01

    A systematic approach was developed for the synthesis of orthophosphates in the laboratory. A set of experiments was designed to investigate the influence of initial calcium and phosphorus concentration on the precipitated phase, nucleation pH and product size distribution at 25°C. Another goal was to characterize the precipitated phase. The investigation was conducted in a batch reactor. The initial molar concentration of calcium chloride and hydrated sodium phosphate solutions was varied from 0.005 to 0.08-mole dm -3 and the solution pH was kept under 7.1. Analysis by powder XRD, FTIR and elemental P/Ca revealed that the crystals precipitated were pure brushite (dicalcium phosphate dihydrate), as expected, except in one experiment in which amorphous calcium phosphate precipitated. The brushite crystals produced had plate-like morphology as investigated by scanning electron microscopy (SEM). The nucleation pH showed a decreasing trend as the concentration of the calcium and phosphorus increased in the reactor, but the volume mean diameter of the crystals and the span of the crystal size distribution did not show any sensitivity to the changes in the initial calcium and phosphorus concentration.

  10. Effects of Silicon on Osteoclast Cell Mediated Degradation, In Vivo Osteogenesis and Vasculogenesis of Brushite Cement

    OpenAIRE

    2015-01-01

    Calcium phosphate cements (CPCs) are being widely used for treating small scale bone defects. Among the various CPCs, brushite (dicalcium phosphate dihydrate, DCPD) cement is widely used due to its superior solubility and ability to form new bone. In the present study, we have studied the physical, mechanical, osteoclast-like-cells differentiation and in vivo osteogenic and vasculogenic properties of silicon (Si) doped brushite cements. Addition of Si did not alter the phase composition of fi...

  11. Determinants of brushite stone formation: a case-control study.

    Directory of Open Access Journals (Sweden)

    Roswitha Siener

    Full Text Available PURPOSE: The occurrence of brushite stones has increased during recent years. However, the pathogenic factors driving the development of brushite stones remain unclear. METHODS: Twenty-eight brushite stone formers and 28 age-, sex- and BMI-matched healthy individuals were enrolled in this case-control study. Anthropometric, clinical, 24 h urinary parameters and dietary intake from 7-day weighed food records were assessed. RESULTS: Pure brushite stones were present in 46% of patients, while calcium oxalate was the major secondary stone component. Urinary pH and oxalate excretion were significantly higher, whereas urinary citrate was lower in patients as compared to healthy controls. Despite lower dietary intake, urinary calcium excretion was significantly higher in brushite stone patients. Binary logistic regression analysis revealed pH>6.50 (OR 7.296; p = 0.035, calcium>6.40 mmol/24 h (OR 25.213; p = 0.001 and citrate excretion <2.600 mmol/24 h (OR 15.352; p = 0.005 as urinary risk factors for brushite stone formation. A total of 56% of patients exhibited distal renal tubular acidosis (dRTA. Urinary pH, calcium and citrate excretion did not significantly differ between patients with or without dRTA. CONCLUSIONS: Hypercalciuria, a diminished citrate excretion and an elevated pH turned out to be the major urinary determinants of brushite stone formation. Interestingly, urinary phosphate was not associated with urolithiasis. The increased urinary oxalate excretion, possibly due to decreased calcium intake, promotes the risk of mixed stone formation with calcium oxalate. Neither dietary factors nor dRTA can account as cause for hypercalciuria, higher urinary pH and diminished citrate excretion. Further research is needed to define the role of dRTA in brushite stone formation and to evaluate the hypothesis of an acquired acidification defect.

  12. Physicochemical characterization of zinc-substituted calcium phosphates

    Indian Academy of Sciences (India)

    DOROTA WALCZYK; DAGMARA MALINA; MILENA KRÓL; KLAUDIA PLUTA; AGNIESZKA SOBCZAK-KUPIEC

    2016-04-01

    Biocompatible and bioactive calcium phosphates can make chemical bonds with living bones. Improvement of their biological and physicochemical properties can be achieved by doping with various ions that are presented in natural apatites of bones. These substitutions influence lattice parameters, structure and morphology of apatites. In recent times great attention has been devoted to zinc ions that are the second most abundant trace element present in bones. Zinc embedded into calcium phosphate may enhance the bone formation and in addition exhibits antifungal and antibacterial properties. Therefore, it is rational to form structures incorporated with this ion. In this paper the incorporation of the Zn ions into natural and synthetic calcium phosphates has been reported.Natural hydroxyapatites (HAs) applied in this study were derived mainly from pork bones whereas both brushite and synthetic were formed using wet chemical methods. Ambient temperature synthesis leads to the formation ofbrushite, whereas the process performed at elevated temperature gives HA. Subsequently, attained structures were modified with Zn ions by using in situ or sorption procedures. Phase composition and morphology of obtained materials were determined by means of X-ray diffractometry, Fourier transform infrared spectroscopy and scanning electron microscopy equipped with energy-dispersive spectroscopy. Introduced XRD patterns depict changes of the crystallinity of HA with the increase in the amount of embedded zinc ions. On the contrary, no changes of the crystallinity were observed for the brushite doped with Zn ions. Morphology of attained powders, visualized using scanningelectron microscopy exemplified structural changes between calcium phosphates conjugated with zinc ions. Many authors report that the addition of small amounts of Zn ions leads to loss of crystallinity and decrease of lattice parameters. Interestingly, upon addition of Zn ions to the natural and synthetic HAp by sorption

  13. Growth and characterization of calcium hydrogen phosphate dihydrate crystals from single diffusion gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Rajendran, K.; Dale Keefe, C. [Department of Chemistry, Cape Breton University, Sydney, Nova Scotia (Canada)

    2010-09-15

    Calcium hydrogen phosphate dihydrate (CaHPO{sub 4}.2H{sub 2}O, CHPD) a dissolved mineral in urine is known to cause renal or bladder stones in both human and animals. Growth of CHPD or brushite using sodium metasilicate gel techniques followed by light and polarizing microscopic studies revealed its structural and morphological details. Crystal identity by powder x-ray diffraction confirmed the FT-IR and FT-Raman spectroscopic techniques as alternate methods for fast analysis of brushite crystals which could form as one type of renal stones. P-O-P asymmetric stretchings in both FT-IR (987.2, 874.1 and 792 cm{sup -1}) and FT-Raman (986.3 cm{sup -1}, 1057.6 cm{sup -1} and 875.2 cm{sup -1}) were found as characteristics of brushite crystals. Differential Scanning Calorimetry (DSC) analysis revealed brushite crystallization purity using gel method by studying their endothermic peaks. This study incorporated a multidisciplinary approach in characterizing CHPD crystals grown in vitro to help formulate prevention or dissolution strategy in controlling urinary stone growth. Initial studies with 0.2 M citric acid ions as controlling agent in the nucleation of brushite crystals further support the presented approach. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Brushite coatings on titanium for orthopedic implants: Studies on deposition and transformation

    Science.gov (United States)

    Kumar, Mukesh

    Hydroxyapatite (HA, Ca5(PO4)3OH) coating on the metallic substrate is expected to assist bone growth and implant integration. However, HA is quite stable in physiological solution and the use of other more reactive calcium phosphate ceramics (CPC) could induce faster bone growth by providing calcium and phosphate ions to the interacting physiological solution. This study utilized a non-line of sight electrodeposition process to achieve brushite (CaHPO4.2H2O) coatings. The uses of potassium or sodium chloride as a conducting electrolyte in the depositing bath enhanced deposition rates and altered the morphology of the coatings. Analysis suggested a strained deposit with sight specific substitution of cations from the conducting electrolyte. Such a deposit (modified brushite) was determined to have CaHPO 4.2H2O and CaY2(1-x)HPO4•2H 2O (x ˜0.95) with Y as Na0 or K. Whereas normal brushite was obtained from unsupported baths. The deposited mass of brushite increased with charge consumed and bonding to the substrate decreased with increasing deposition time. Though inconclusive. in-situ studies on electrodeposition did not rule out the possibility of ionic species responsible for the deposit. Transformations of both forms of brushite were investigated in calcium free Hank's type simulated body fluid. Modified brushite showed periodic appearance of freshly precipitated, but poorly crystalline HA, without the benefit of monetite (CaHPO4) as an intermediate. However, normal brushite transformation showed nonstoichiometric HA with monetite as an intermediate. Normal brushite demonstrated a slower transformation to HA when compared to the transformation kinetics of modified brushite. It is shown that lattice strain due to localized ion incorporation could be used to after the properties of brushite coatings to adjust the kinetics of transformation and indirectly the amount of calcium and phosphate ions released into the surrounding.

  15. Effect of cold-setting calcium- and magnesium phosphate matrices on protein expression in osteoblastic cells.

    Science.gov (United States)

    Ewald, Andrea; Helmschrott, Kerstin; Knebl, Georg; Mehrban, Nazia; Grover, Liam M; Gbureck, Uwe

    2011-02-01

    Bone loss due to accidents or tissue diseases requires replacement of the structure by either autografts, allografts, or artificial materials. Reactive cements, which are based on calcium phosphate chemistry, are commonly used in nonload bearing areas such as the craniofacial region. Some of these materials are resorbed by the host under physiological conditions and replaced by bone. The aim of this study was to test different calcium and magnesium cement composites in vitro for their use as bone substitution material. Phase composition of calcium deficient hydroxyapatite (Ca(9) (PO(4) )(5) HPO(4) OH), brushite (CaHPO(4) ·2H(2) O), and struvite (MgNH(4) PO(4) ·6H(2) O) specimens has been determined by means of X-ray diffraction, and compressive strength was measured. Cell growth and activity of osteoblastic cells (MG 63) on the different surfaces was determined, and the expression of bone marker proteins was analyzed by western blotting. Cell activity normalized to cell number revealed higher activity of the osteoblasts on brushite and struvite when compared to hydroxyapatite and also the expression of osteoblastic marker proteins was highest on brushite scaffolds. While brushite sets under acidic conditions, formation of struvite occurs under physiological pH, similar to hydroxyapatite cements, providing the possibility of additional modifications with proteins or other active components.

  16. Development and characterisation of injectable calcium phosphate cements for use in vertebroplasty

    OpenAIRE

    2002-01-01

    The global objective of this thesis was to understand how the starting components of brushite cements influence the cement properties relevant for its use in vertebroplasty. Therefore, this work focussed on the following cement properties : mechanical strength, X-ray opacity and heat release upon setting. To carry out the global objective, a test protocol was first developed to characterise the mechanical properties of calcium phosphate cements. The Mohr's circles representation allowed to un...

  17. Development and characterisation of injectable calcium phosphate cements for use in vertebroplasty

    OpenAIRE

    2007-01-01

    The global objective of this thesis was to understand how the starting components of brushite cements influence the cement properties relevant for its use in vertebroplasty. Therefore, this work focussed on the following cement properties : mechanical strength, X-ray opacity and heat release upon setting. To carry out the global objective, a test protocol was first developed to characterise the mechanical properties of calcium phosphate cements. The Mohr's circles representation allowed to un...

  18. Water-Soluble Cellulose Derivatives Are Sustainable Additives for Biomimetic Calcium Phosphate Mineralization

    OpenAIRE

    2016-01-01

    The effect of cellulose-based polyelectrolytes on biomimetic calcium phosphate mineralization is described. Three cellulose derivatives, a polyanion, a polycation, and a polyzwitterion were used as additives. Scanning electron microscopy, X-ray diffraction, IR and Raman spectroscopy show that, depending on the composition of the starting solution, hydroxyapatite or brushite precipitates form. Infrared and Raman spectroscopy also show that significant amounts of nitrate ions are incorporated i...

  19. Synthesis of nanocrystalline calcium phosphate in microemulsion--effect of nature of surfactants.

    Science.gov (United States)

    Singh, Sujata; Bhardwaj, Pallavi; Singh, V; Aggarwal, S; Mandal, U K

    2008-03-01

    Nanosized calcium phosphate (CP) powders have been synthesized by an inverse microemulsion system using kerosene as the oil phase, a cationic surfactant Aliquat 336, a non-ionic surfactant Tween 20 and their mixture and aqueous solutions of calcium nitrate tetrahydrate and biammonium hydrogen phosphate as the water phase. It has been found that the nature of surfactants played an important role to regulate the size and morphologies of the calcium phosphate nanoparticles. The cationic surfactant Aliquat 336 has been found to regulate the nucleation and crystal growth. The synthesized powders have been comprehensively characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). Our results show that the brushite (DCPD) is the major phase comprising the calcium phosphate nanoparticles. In mixed surfactants mediated system a morphological controlled highly crystalline particles have been synthesized. Further, the role of Aliquat 336 has been established and a plausible synthetic mechanism has been proposed.

  20. Growth units and nucleation: The case of calcium phosphates

    Science.gov (United States)

    Boistelle, Roland; Lopez-Valero, Isabel

    1990-05-01

    Calcium phosphates are precipitated at 37°C from solutions the pH of which ranges from 5.0 to 11.0. Despite the fact that the supersaturations of hydroxyapatite HAP, octocalcium phosphate OCP and brushite B are often in the order HAP≫OCP≫B, brushite nucleates more easily than OCP and HAP at low pH, while OCP nucleates more easily than HAP at mean to high pH. These facts cannot be explained, as usually, by the only differences in the surface free energies of the three solid phases. On the other hand, they may be explained by assuming that the values of the kinetic coefficients change as a function of the concentration in the proper growth units which have to integrate in the nuclei of either phase. In the model we propose, the kinetic coefficients of OCP and HAP are smaller than that of B by 10 and 18 orders of magnitude at pH=6.5, differences which reduce to 3 orders of magnitude at pH=10.0. Accordingly, nucleation of OCP and HAP is favoured with increasing pH.

  1. Calcium phosphate nucleation on surface-modified PTFE membranes.

    Science.gov (United States)

    Grøndahl, Lisbeth; Cardona, Francisco; Chiem, Khang; Wentrup-Byrne, Edeline; Bostrom, Thor

    2003-06-01

    Highly porous PTFE membranes are currently being used in facial reconstructive surgery. The present study aims at improving this biomaterial through creating a more bioactive surface by introducing ionic groups onto the surface. The unmodified PTFE membrane does not induce inorganic growth after immersion in simulated body fluid (SBF) for up to 4 weeks. Copolymeric grafting with acrylic acid (AAc) by means of gamma irradiation and subsequent in vitro testing in SBF reveals that this copolymer initially acts as an ion-exchange material and subsequently induces growth of a calcium phosphate phase (Ca/P=2.7) when large amounts (15%) of pAAc are introduced onto the membrane surface. This copolymer is not expected to function well from a biomaterials perspective since SEM showed the pores on the surface to be partly blocked. In contrast, the surface of monoacryloxyethyl phosphate (MAEP)-modified samples is altered at a molecular level only. Yet the modified materials are able to induce calcium phosphate nucleation when the external surface coverage is 44% or above. The initial inorganic growth on these membranes in SBF has a (Ca+Mg)/P ratio of 1.1 (presumably Brushite or Monetite). The secondary growth, possibly calcium-deficient apatite or tricalcium phosphate, has a (Ca+Mg)/P ratio of 1.5. This result is a promising indicator of a bioactive biomaterial.

  2. Phase composition, mechanical performance and in vitro biocompatibility of hydraulic setting calcium magnesium phosphate cement.

    Science.gov (United States)

    Klammert, Uwe; Reuther, Tobias; Blank, Melanie; Reske, Isabelle; Barralet, Jake E; Grover, Liam M; Kübler, Alexander C; Gbureck, Uwe

    2010-04-01

    Brushite (CaHPO(4) x 2H(2)O)-forming calcium phosphate cements are of great interest as bone replacement materials because they are resorbable in physiological conditions. However, their short setting times and low mechanical strengths limit broad clinical application. In this study, we showed that a significant improvement of these properties of brushite cement could be achieved by the use of magnesium-substituted beta-tricalcium phosphate with the general formula Mg(x)Ca((3-x))((PO(4))(2) with 0 cement reactants. The incorporation of magnesium ions increased the setting times of cements from 2 min for a magnesium-free matrix to 8-11 min for Mg(2.25)Ca(0.75)(PO(4))(2) as reactant. At the same time, the compressive strength of set cements was doubled from 19 MPa to more than 40 MPa after 24h wet storage. Magnesium ions were not only retarding the setting reaction to brushite but were also forming newberyite (MgHPO(4) x 3H(2)O) as a second setting product. The biocompatibility of the material was investigated in vitro using the osteoblast-like cell line MC3T3-E1. A considerable increase of cell proliferation and expression of alkaline phosphatase, indicating an osteoblastic differentiation, could be noticed. Scanning electron microscopy analysis revealed an obvious cell growth on the surface of the scaffolds. Analysis of the culture medium showed minor alterations of pH value within the physiological range. The concentrations of free calcium, magnesium and phosphate ions were altered markedly due to the chemical solubility of the scaffolds. We conclude that the calcium magnesium phosphate (newberyite) cements have a promising potential for their use as bone replacement material since they provide a suitable biocompatibility, an extended workability and improved mechanical performance compared with brushite cements.

  3. 21 CFR 582.5217 - Calcium phosphate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Calcium phosphate. 582.5217 Section 582.5217 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) ANIMAL... Supplements 1 § 582.5217 Calcium phosphate. (a) Product. Calcium phosphate (mono-, di-, and tribasic)....

  4. 21 CFR 582.1217 - Calcium phosphate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Calcium phosphate. 582.1217 Section 582.1217 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) ANIMAL... Additives § 582.1217 Calcium phosphate. (a) Product. Calcium phosphate (mono-, di-, and tribasic)....

  5. 21 CFR 182.1217 - Calcium phosphate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Calcium phosphate. 182.1217 Section 182.1217 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR... Substances § 182.1217 Calcium phosphate. (a) Product. Calcium phosphate (mono-, di-, and tribasic)....

  6. The Effects of Crystal Phase and Particle Morphology of Calcium Phosphates on Proliferation and Differentiation of Human Mesenchymal Stromal Cells.

    Science.gov (United States)

    Danoux, Charlène; Pereira, Daniel; Döbelin, Nicola; Stähli, Christoph; Barralet, Jake; van Blitterswijk, Clemens; Habibovic, Pamela

    2016-07-01

    Calcium phosphate (CaP) ceramics are extensively used for bone regeneration; however, their clinical performance is still considered inferior to that of patient's own bone. To improve the performance of CaP bone graft substitutes, it is important to understand the effects of their individual properties on a biological response. The aim of this study is to investigate the effects of the crystal phase and particle morphology on the behavior of human mesenchymal stromal cells (hMSCs). To study the effect of the crystal phase, brushite, monetite, and octacalcium phosphate (OCP) are produced by controlling the precipitation conditions. Brushite and monetite are produced as plate-shaped and as needle-shaped particles, to further investigate the effect of particle morphology. Proliferation of hMSCs is inhibited on OCP as compared to brushite and monetite in either morphology. Brushite needles consistently show the lowest expression of most osteogenic markers, whereas the expression on OCP is in general high. There is a trend toward a higher expression of the osteogenic markers on plate-shaped than on needle-shaped particles for both brushite and monetite. Within the limits of CaP precipitation, these data indicate the effect of both crystal phase and particle morphology of CaPs on the behavior of hMSCs.

  7. Influence of raw powder granulometry on the mechanical properties of a calcium phosphate bone cement

    Energy Technology Data Exchange (ETDEWEB)

    Pittet, C. [Swiss Federal Inst. of Tech., Lausanne (Switzerland). Lab. de Technologie des Poudres; Hopital Orthopedique de la Suisse Romande, Lausanne (Switzerland); Grasso, P.; Lemaitre, J. [Swiss Federal Inst. of Tech., Lausanne (Switzerland). Lab. de Technologie des Poudres

    2002-07-01

    Brushite cement is a calcium phosphate cement obtained by mixing three powders with water. Starting powders are monocalcium phosphate monohydrate (MCPM), calcium sulfate hemihydrate (CSH) and {beta}-tricalcium phosphate ({beta}-TCP). The main phase obtained after setting is brushite (DCPD). The goal of this work was to mill the starting powders to obtain a finer and more homogeneous microstructure after setting, in order to enhance the mechanical properties of the cement. All three powders were milled and freeze-dried. The median diameters passed from 70.5 to 6.2 {mu}m for MCPM, 27.2 to 1.1 {mu}m for CSH, 2.4 to 1.5 {mu}m for {beta}-TCP. Specific surface areas of the powders increased on milling. Attrition of MCPM and CSH appeared to be beneficial to the maximum stresses the set cement can withstand. Cements prepared with raw powders showed 1.4 MPa indirect tensile strength and 4.4 MPa compressive strength. With milled MCPM and CSH, those values reached 4.1 and 22.1 MPa respectively. After these benefits, we tried to use the milled {beta}-TCP expecting further enhancement. To ensure wetting of all three powders and to keep the same paste rheology, the liquid/solid ratio had to be increased. The indirect tensile strength was seen to decrease by a factor of 3 when three milled powders were used at the same time. SEM of the fracture surfaces showed that milled {beta}-TCP formed clusters that did not react to form brushite. Lowering the maximum indirect tension stress is due to the fact that less brushite was formed, and to a higher porosity in the final product (mainly due to the higher liquid/solid ratio). (orig.)

  8. Cytocompatibility of brushite and monetite cell culture scaffolds made by three-dimensional powder printing.

    Science.gov (United States)

    Klammert, U; Reuther, T; Jahn, C; Kraski, B; Kübler, A C; Gbureck, U

    2009-02-01

    This study investigated the cytocompatibility of low-temperature direct 3-D printed calcium phosphate scaffolds in vitro. The fabrication of the scaffolds was performed with a commercial 3-D powder printing system. Diluted phosphoric acid was printed into tricalcium phosphate powder, leading to the formation of dicalcium phosphate dihydrate (brushite). Hydrothermal conversion of the brushite matrices led to the formation of dicalcium phosphate anhydrous (monetite). The biocompatibility was investigated using the osteoblastic cell line MC3T3-E1. Cell viability and the expression of alkaline phosphatase served as parameters. The culture medium was analyzed for pH value, concentration of free calcium and phosphate ions and osteocalcin. Both types of scaffolds showed a considerable increase of cell proliferation and viability; the monetite matrices were a little inferior compared with the brushite ones. The activity of alkaline phosphatase showed a similar pattern. Optical and electron microscopy revealed an obvious cell growth on the surface of both materials. Analysis of the culture medium showed minor alterations of pH value within the physiological range. The concentrations of free calcium and phosphate ions were obviously different among brushite and monetite cultures, due to their different solubility. The content of osteocalcin of the culture medium was reduced by the printed scaffolds due to adsorption. We conclude that the powder printed brushite and monetite matrices have a suitable biocompatibility for their use as cell culture scaffolds. Both materials enable osteoblastic cells in vitro to proliferate and differentiate due to the expression of typical osteoblastic markers.

  9. Calcium phosphate polymer hybrid materials

    OpenAIRE

    2011-01-01

    Calcium phosphate (CaP) is of strong interest to the medical field because of its potential for bone repair, gene transfection, etc.1-3 Nowadays, the majority of the commercially available materials are fabricated via “classical” materials science approaches, i.e. via high temperature or high pressure approaches, from rather poorly defined slurries, or from organic solvents.3,4 Precipitation of inorganics with (polymeric) additives from aqueous solution on the other hand enables the synthesis...

  10. Sintering of calcium phosphate bioceramics.

    Science.gov (United States)

    Champion, E

    2013-04-01

    Calcium phosphate ceramics have become of prime importance for biological applications in the field of bone tissue engineering. This paper reviews the sintering behaviour of these bioceramics. Conventional pressureless sintering of hydroxyapatite, Ca10(PO4)6(OH)2, a reference compound, has been extensively studied. Its physico-chemistry is detailed. It can be seen as a competition between two thermally activated phenomena that proceed by solid-state diffusion of matter: densification and grain growth. Usually, the objective is to promote the first and prevent the second. Literature data are analysed from sintering maps (i.e. grain growth vs. densification). Sintering trajectories of hydroxyapatite produced by conventional pressureless sintering and non-conventional techniques, including two-step sintering, liquid phase sintering, hot pressing, hot isostatic pressing, ultrahigh pressure, microwave and spark plasma sintering, are presented. Whatever the sintering technique may be, grain growth occurs mainly during the last step of sintering, when the relative bulk density reaches 95% of the maximum value. Though often considered very advantageous, most assisted sintering techniques do not appear very superior to conventional pressureless sintering. Sintering of tricalcium phosphate or biphasic calcium phosphates is also discussed. The chemical composition of calcium phosphate influences the behaviour. Similarly, ionic substitutions in hydroxyapatite or in tricalcium phosphate create lattice defects that modify the sintering rate. Depending on their nature, they can either accelerate or slow down the sintering rate. The thermal stability of compounds at the sintering temperature must also be taken into account. Controlled atmospheres may be required to prevent thermal decomposition, and flash sintering techniques, which allow consolidation at low temperature, can be helpful.

  11. Effect of solute concentration on fibroin regulated biomineralization of calcium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Kong Xiangdong [Biomaterials Laboratory, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Institute of Biochemistry, Zhejiang Sci-Tech University, Hangzhou 310018 (China); Sun Xiaodan [Biomaterials Laboratory, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Cui Fuzhai [Biomaterials Laboratory, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China)]. E-mail: cuifz@mail.tsinghua.edu.cn; Ma Chen [Biomaterials Laboratory, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China)

    2006-05-15

    In this paper we used UV/Visible method to study the effect of solute concentration on fibroin regulated biomineralization of calcium phosphate. During the reaction process, ultraviolet-visible spectrophotometer was used to track the extinction in the reaction solution. It is found that kinetics of the biomineralization can be strongly affected by the presence of fibroin. Fibroin with higher concentration has more positive effect on the biomineralization process. Under the appropriate reaction conditions, wave crest and wave trough appear in the kinetic curves of fibroin biomineralization. The wave crest and wave trough phenomenon is mainly related with the process of phase separation. X-ray Diffraction (XRD) result shows the calcium phosphate before the wave trough is mainly amorphous calcium phosphate, while after the wave trough crystal of hydroxyapatite (HA) and brushite (DCPD) are the mainly ingredients.

  12. Preparation of tricalcium phosphate/calcium pyrophosphate structures via rapid prototyping.

    Science.gov (United States)

    Gbureck, Uwe; Hölzel, Tanja; Biermann, Isabell; Barralet, Jake E; Grover, Liam M

    2008-04-01

    Custom made tricalcium phosphate/calcium pyrophosphate bone substitutes with a well-defined architecture were fabricated in this study using 3D powder printing with tricalcium phosphate (TCP) powder and a liquid phase of phosphoric acid. The primary formed matrix of dicalcium phosphate dihydrate (DCPD, brushite) was converted in a second step to calcium pyrophosphate (CPP) by heat treatment in the temperature range 1,100-1,300 degrees C. The structures exhibited compressive strengths between 0.8 MPa and 4 MPa after sintering at 1,100-1,250 degrees C, higher strengths were obtained by increasing the amount of pyrophosphate formed in the matrix due to a post-hardening regime prior sintering as well as by the formation of a glass phase from TCP and calcium pyrophosphate above 1,280 degrees C, which resulted in a strong densification of the samples and compressive strength of >40 MPa.

  13. In vivo degradation of low temperature calcium and magnesium phosphate ceramics in a heterotopic model.

    Science.gov (United States)

    Klammert, Uwe; Ignatius, Anita; Wolfram, Uwe; Reuther, Tobias; Gbureck, Uwe

    2011-09-01

    Bone replacement using synthetic and degradable materials is desirable in various clinical conditions. Most applied commercial materials are based on hydroxyapatite, which is not chemically degradable under physiological conditions. Here we report the effect of a long-term intramuscular implantation regime on the dissolution of various low temperature calcium and magnesium phosphate ceramics in vivo. The specimens were analysed by consecutive radiographs, micro-computed tomography scans, compressive strength testing, scanning electron microscopy and X-ray diffractometry. After 15months in vivo, the investigated materials brushite (CaHPO(4)·2H(2)O), newberyite (MgHPO(4)·3H(2)O), struvite (MgNH(4)PO(4)·6H(2)O) and hydroxyapatite (Ca(9)(PO(4))(5)HPO(4)OH) showed significant differences regarding changes of their characteristics. Struvite presented the highest loss of mechanical performance (95%), followed by newberyite (67%) and brushite (41%). This was accompanied by both a distinct extent of cement dissolution as well as changes of the phase composition of the retrieved cement implants. While the secondary phosphate phases (brushite, newberyite, struvite) completely dissolved, re-precipitates of whitlockite and octacalcium phosphate were formed in either particulate or whisker-like morphology. Furthermore, for the first time the possibility of a macropore-free volume degradation mechanism of bioceramics was demonstrated.

  14. Synthesis of spherical calcium phosphate particles for dental and orthopedic applications.

    Science.gov (United States)

    Bohner, Marc; Tadier, Solène; van Garderen, Noémie; de Gasparo, Alex; Döbelin, Nicola; Baroud, Gamal

    2013-01-01

    Calcium phosphate materials have been used increasingly in the past 40 years as bone graft substitutes in the dental and orthopedic fields. Accordingly, numerous fabrication methods have been proposed and used. However, the controlled production of spherical calcium phosphate particles remains a challenge. Since such particles are essential for the synthesis of pastes and cements delivered into the host bone by minimally-invasive approaches, the aim of the present document is to review their synthesis and applications. For that purpose, production methods were classified according to the used reagents (solutions, slurries, pastes, powders), dispersion media (gas, liquid, solid), dispersion tools (nozzle, propeller, sieve, mold), particle diameters of the end product (from 10 nm to 10 mm), and calcium phosphate phases. Low-temperature calcium phosphates such as monetite, brushite or octacalcium phosphate, as well as high-temperature calcium phosphates, such as hydroxyapatite, β-tricalcium phosphate or tetracalcium phosphate, were considered. More than a dozen production methods and over hundred scientific publications were discussed.

  15. Synthesis of spherical calcium phosphate particles for dental and orthopedic applications

    Science.gov (United States)

    Bohner, Marc; Tadier, Solène; van Garderen, Noémie; de Gasparo, Alex; Döbelin, Nicola; Baroud, Gamal

    2013-01-01

    Calcium phosphate materials have been used increasingly in the past 40 years as bone graft substitutes in the dental and orthopedic fields. Accordingly, numerous fabrication methods have been proposed and used. However, the controlled production of spherical calcium phosphate particles remains a challenge. Since such particles are essential for the synthesis of pastes and cements delivered into the host bone by minimally-invasive approaches, the aim of the present document is to review their synthesis and applications. For that purpose, production methods were classified according to the used reagents (solutions, slurries, pastes, powders), dispersion media (gas, liquid, solid), dispersion tools (nozzle, propeller, sieve, mold), particle diameters of the end product (from 10 nm to 10 mm), and calcium phosphate phases. Low-temperature calcium phosphates such as monetite, brushite or octacalcium phosphate, as well as high-temperature calcium phosphates, such as hydroxyapatite, β-tricalcium phosphate or tetracalcium phosphate, were considered. More than a dozen production methods and over hundred scientific publications were discussed. PMID:23719177

  16. 21 CFR 182.8217 - Calcium phosphate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Calcium phosphate. 182.8217 Section 182.8217 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR... phosphate. (a) Product. Calcium phosphate (mono-, di-, and tribasic). (b) Conditions of use. This...

  17. Modeling vancomycin release kinetics from microporous calcium phosphate ceramics comparing static and dynamic immersion conditions.

    Science.gov (United States)

    Gbureck, Uwe; Vorndran, Elke; Barralet, Jake E

    2008-09-01

    The release kinetics of vancomycin from calcium phosphate dihydrate (brushite) matrices and polymer/brushite composites were compared using different fluid replacement regimes, a regular replacement (static conditions) and a continuous flow technique (dynamic conditions). The use of a constantly refreshed flowing resulted in a faster drug release due to a constantly high diffusion gradient between drug loaded matrix and the eluting medium. Drug release was modeled using the Weibull, Peppas and Higuchi equations. The results showed that drug liberation was diffusion controlled for the ceramics matrices, whereas ceramics/polymer composites led to a mixed diffusion and degradation controlled release mechanism. The continuous flow technique was for these materials responsible for a faster release due to an accelerated polymer degradation rate compared with the regular fluid replacement technique.

  18. Growth of calcium phosphates on magnesium substrates for corrosion control in biomedical applications via immersion techniques.

    Science.gov (United States)

    Shadanbaz, Shaylin; Walker, Jemimah; Staiger, Mark P; Dias, George J; Pietak, Alexis

    2013-01-01

    Magnesium (Mg) has been suggested as a revolutionary biodegradable replacement for current permanent metals used in orthopedic applications. Current investigations concentrate on the control of the corrosion rate to match bone healing. Calcium phosphate coatings have been a recent focus of these investigations through various coating protocols. Within this investigation, an in situ crystallization technique was utilized as an inexpensive and relatively simple method to produce a brushite and monetite coating on pure Mg. Coatings were characterized using energy dispersive spectroscopy, glancing angle X-ray diffraction and field emission scanning electron microscopy. Corrosion protection properties of the coatings were assessed in physiological buffers, Earles balanced salt solution, minimum essential media, and minimum essential media containing serum albumin, over a 4-week period. Using this novel coating protocol, our findings indicate brushite and monetite coated Mg to have significant corrosive protective effects when compared with its uncoated counterpart whilst maintaining high coating substrate adhesion, homogeneity, and reproducibility.

  19. Chemical synthesis and stabilization of magnesium substituted brushite

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Donghyun [Department of Biomedical Engineering, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul 156-756 (Korea, Republic of); Kumta, Prashant N., E-mail: pkumta@pitt.edu [Department of Bioengineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Mechanical Engineering and Materials Sceince, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Chemical and Petroleum Engineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States)

    2010-08-30

    Hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) is the most ubiquitous calcium phosphate phase used in implant coatings and more recently in gene/drug delivery applications due to its chemical stability under normal physiological conditions (37 deg. C, pH {approx} 7.5, 1 atm.). However, different calcium phosphate phases, such as brushite (CaH(PO{sub 4}){center_dot}2(H{sub 2}O)) and tricalcium phosphate (Ca{sub 3}(PO{sub 4}){sub 2}) which are thermodynamically unstable under physiological conditions are also being explored for biomedical applications. One way of stabilizing these phases under physiological conditions is to introduce magnesium to substitute for calcium in the brushite lattice. The role of magnesium as a stabilizing agent for synthesizing brushite under physiological conditions at room temperature has been studied. Chemical analysis, Fourier transform infrared spectroscopy and X-ray diffraction have also been conducted to validate the formation of magnesium substituted brushite under physiological conditions.

  20. Constant composition dissolution of mixed phases. II. Selective dissolution of calcium phosphates.

    Science.gov (United States)

    Tang, Ruikang; Hass, Michael; Wu, Wenju; Gulde, Stacey; Nancollas, George H

    2003-04-15

    Characterization of the dissolution kinetics of individual synthetic and biological calcium phosphates is of considerable importance since these phases often coexist in biological minerals. The constant composition method has been used to study the dissolution kinetics of a series of synthetic calcium phosphates, brushite (DCPD), beta-tricalcium phosphate (TCP), octacalcium phosphate (OCP), hydroxyapatite (HAP), and carbonated apatite (CAP) in the presence and absence of citric acid, as a function of pH and thermodynamic driving force. While citric acid markedly accelerates the dissolution of TCP, HAP dissolution is significantly inhibited. Moreover, this additive has almost no influence on the dissolution of DCPD, OCP, and CAP. Dual constant composition dissolution studies of mixed calcium phosphates in the presence of citric acid have also been made. Another factor, pH, also plays an important role in the dissolution of these calcium phosphates. In suspensions of calcium phosphate mixtures, specific phases can be selectively dissolved by changing experimental parameters such as pH and the presence of rate modifiers. This result has important applications for the dissolution control of dental hard tissues such as dentin, enamel, and calculus.

  1. Stability and mutual conversion of enamel apatite and brushite at 20 degrees C as a function of pH of the aqueous phase.

    Science.gov (United States)

    Larsen, M J; Jensen, S J

    1989-01-01

    By calculation, apatite is more soluble than brushite at low pH and less soluble at high pH. Apatite, therefore should be able to transform spontaneously to brushite at low pH and brushite to apatite at high pH. The aim was to describe this mutual conversion as related to the aqueous phase composition. Powdered enamel, brushite or 1:1 mixtures of the two salts were suspended in distilled water for up to 12 weeks at 20 degrees C, pH was adjusted to 4, 5, 6, 7, 8, 9 or 10 by drops of perchloric acid or potassium hydroxide. The calcium and the phosphate concentrations and pH were determined, and the nature of the calcium phosphate powder was examined by X-ray diffraction. At pH 8 and above, brushite was invariably converted to apatite, whilst it was transformed to octacalcium phosphate at pH 7. In the pH range 6-4 brushite was not converted to apatite and enamel apatite was not transformed to brushite spontaneously within 2 months. In the enamel apatite suspensions, the apatite ion product altered with pH, which explained why apatite did not transform to brushite at pH 5-4. At pH 3.7, however, the enamel apatite was converted to brushite. No transformation of apatite to brushite was identified in apatite-brushite mixtures at pH 6-4. Supplementary experiments showed that ethanol, used as an agent for removal of water, salted out the water-free dicalcium phosphate, monetite.

  2. Application of Calcium Phosphate Materials in Dentistry

    Directory of Open Access Journals (Sweden)

    Jabr S. Al-Sanabani

    2013-01-01

    Full Text Available Calcium phosphate materials are similar to bone in composition and in having bioactive and osteoconductive properties. Calcium phosphate materials in different forms, as cements, composites, and coatings, are used in many medical and dental applications. This paper reviews the applications of these materials in dentistry. It presents a brief history, dental applications, and methods for improving their mechanical properties. Notable research is highlighted regarding (1 application of calcium phosphate into various fields in dentistry; (2 improving mechanical properties of calcium phosphate; (3 biomimetic process and functionally graded materials. This paper deals with most common types of the calcium phosphate materials such as hydroxyapatite and tricalcium phosphate which are currently used in dental and medical fields.

  3. Procedure for the study of acidic calcium phosphate precursor phases in enamel mineral formation.

    Science.gov (United States)

    Siew, C; Gruninger, S E; Chow, L C; Brown, W E

    1992-02-01

    Considerable evidence suggests that an acidic calcium phosphate, such as octacalcium phosphate (OCP) or brushite, is involved as a precursor in enamel and other hard tissue formation. Additionally, there is in vitro evidence suggesting that fluoride accelerates and magnesium inhibits the hydrolysis of OCP to hydroxyapatite (OHAp). As the amount of OCP or brushite in enamel cannot be measured directly in the presence of an excess of hydroxyapatite, a procedure was developed that allows for their indirect in vivo quantification as pyrophosphate. This permits study of the effects of fluoride and magnesium ions on enamel mineral synthesis. Rat incisor calcium phosphate was labeled by intraperitoneal injection of NaH2(32)PO4. The rats were then subjected to various fluoride and magnesium treatments with subcutaneous implanted osmotic pumps. They were then killed at predetermined intervals; the nascent sections of the incisors were collected, cleaned, and pyrolyzed at 500 degrees C for 48 hours to convert acidic calcium phosphates to calcium pyrophosphate; the pyrophosphate was separated from orthophosphate by anion-exchange chromatography; and the resulting fractions were counted by liquid scintillation spectrometry. The activities of the pyro- and orthophosphate fractions were used to calculate the amount of acidic calcium phosphate present in the nascent mineral. The results demonstrated that the percentage of radioactive pyrophosphate in nascent incisors decreased with time, with increasing serum F- concentration, and with decreasing serum magnesium content. The technique described here should prove to be a powerful new tool for studying the effects of various agents on biological mineral formation.

  4. Growth and Characterization of Agar Gel Grown Brushite Crystals

    Directory of Open Access Journals (Sweden)

    V. B. Suryawanshi

    2014-01-01

    Full Text Available Brushite [CaHPO4·2H2O] or calcium hydrogen phosphate dihydrate (CHPD also known as urinary crystal is a stable form of calcium phosphate. The brushite crystals were grown by single and double diffusion techniques in agar-agar gel at room temperature. Effects of different growth parameters were discussed in single diffusion and double diffusion techniques. Good quality star, needle, platy, rectangular, and prismatic shaped crystals in single diffusion and nuclei with dendritic growth were obtained in double diffusion. These grown nuclei were characterized by scanning electron microscopy (SEM, Fourier transform infrared (FTIR spectroscopy, X-ray diffraction (XRD, and thermogravimetric analysis (TGA. SEM has shown the different morphologies of crystals; FTIR has confirmed the presence of functional groups; crystalline nature was supported by XRD, whereas the TGA indicates total 24.68% loss in weight and formation of stable calcium pyrophosphate (Ca2P2O7 at 500°C.

  5. Biological responses of brushite-forming Zn- and ZnSr- substituted beta-tricalcium phosphate bone cements.

    Science.gov (United States)

    Pina, S; Vieira, S I; Rego, P; Torres, P M C; da Cruz e Silva, O A B; da Cruz e Silva, E F; Ferreira, J M F

    2010-09-07

    The core aim of this study was to investigate zinc (Zn)- and zinc and strontium (ZnSr)-containing brushite-forming beta-tricalcium phosphate (TCP) cements for their effects on proliferation and differentiation of osteoblastic-like cells (MC3T3-E1 cell line) as well as for their in vivo behaviour in trabecular bone cylindrical defects in a pilot study. In vitro proliferation and maturation responses of MC3T3-E1 osteoblastic-like cells to bone cements were studied at the cellular and molecular levels. The Zn- and Sr-containing brushite cements were found to stimulate pre-osteoblastic proliferation and osteoblastic maturation. Indeed, MC3T3-E1 cells exposed to the powdered cements had increased proliferative rates and higher adhesiveness capacity, in comparison to control cells. Furthermore, they exhibited higher alkaline phosphatase (ALP) activity and increased Type-I collagen secretion and fibre deposition into the extracellular matrix. Proliferative and collagen deposition properties were more evident for cells grown in cements doped with Sr. The in vivo osteoconductive propertiesof the ZnCPC and ZnSrCPC cements were also pursued. Histological and histomorphometric analyses were performed at 1 and 2 months after implantation, using carbonated apatite cement (Norian SRS) as control. There was no evidence of cement-induced adverse foreign body reactions, and furthermore ZnCPC and ZnSrCPC cements revealed better in vivo performance in comparison to the control apatite cement. Additionally, the presence of both zinc and strontium resulted in the highest rate of new bone formation. These novel results indicate that the investigated ZnCPC and ZnSrCPC cements are both biocompatible and osteoconductive, being good candidate materials to use as bone substitutes.

  6. Biological responses of brushite-forming Zn- and ZnSr- substituted beta-tricalcium phosphate bone cements

    Directory of Open Access Journals (Sweden)

    S Pina

    2010-09-01

    Full Text Available The core aim of this study was to investigate zinc (Zn- and zinc and strontium (ZnSr-containing brushite-forming beta-tricalcium phosphate (TCP cements for their effects on proliferation and differentiation of osteoblastic-like cells (MC3T3-E1 cell line as well as for their in vivo behaviour in trabecular bone cylindrical defects in a pilot study. In vitro proliferation and maturation responses of MC3T3-E1 osteoblastic-like cells to bone cements were studied at the cellular and molecular levels. The Zn- and Sr-containing brushite cements were found to stimulate pre-osteoblastic proliferation and osteoblastic maturation. Indeed, MC3T3-E1 cells exposed to the powdered cements had increased proliferative rates and higher adhesiveness capacity, in comparison to control cells. Furthermore, they exhibited higher alkaline phosphatase (ALP activity and increased Type-I collagen secretion and fibre deposition into the extracellular matrix. Proliferative and collagen deposition properties were more evident for cells grown in cements doped with Sr. The in vivo osteoconductive propertiesof the ZnCPC and ZnSrCPC cements were also pursued. Histological and histomorphometric analyses were performed at 1 and 2 months after implantation, using carbonated apatite cement (Norian SRS® as control. There was no evidence of cement-induced adverse foreign body reactions, and furthermore ZnCPC and ZnSrCPC cements revealed better in vivo performance in comparison to the control apatite cement. Additionally, the presence of both zinc and strontium resulted in the highest rate of new bone formation. These novel results indicate that the investigated ZnCPC and ZnSrCPC cements are both biocompatible and osteoconductive, being good candidate materials to use as bone substitutes.

  7. Polarized infrared reflectance spectra of brushite (CaHPO4·2H2O) crystal investigation of the phosphate stretching modes.

    Science.gov (United States)

    Mevellec, Jean-Yves; Quillard, Sophie; Deniard, Philippe; Mekmene, Omar; Gaucheron, Frédéric; Bouler, Jean-Michel; Buisson, Jean-Pierre

    2013-07-01

    Polarized infrared (IR) reflectance measurements at near-normal incidence were recorded from the ac-plane of a monoclinic brushite (CaHPO4·2H2O) crystal in the 800-1200 cm(-1) spectral range (P-O stretching modes). The adjustment of these data, on the basis of a dispersion analysis (DA) model for monoclinic case, allowed the determination of oscillators parameters for the four P-O stretching observed modes of the phosphate group.

  8. Polarized infrared reflectance spectra of brushite (CaHPO4ṡ2H2O) crystal investigation of the phosphate stretching modes

    Science.gov (United States)

    Mevellec, Jean-Yves; Quillard, Sophie; Deniard, Philippe; Mekmene, Omar; Gaucheron, Frédéric; Bouler, Jean-Michel; Buisson, Jean-Pierre

    2013-07-01

    Polarized infrared (IR) reflectance measurements at near-normal incidence were recorded from the ac-plane of a monoclinic brushite (CaHPO4ṡ2H2O) crystal in the 800-1200 cm-1 spectral range (P-O stretching modes). The adjustment of these data, on the basis of a dispersion analysis (DA) model for monoclinic case, allowed the determination of oscillators parameters for the four P-O stretching observed modes of the phosphate group.

  9. Preparation and mechanical property of core-shell type chitosan/calcium phosphate composite fiber

    Energy Technology Data Exchange (ETDEWEB)

    Matsuda, Atsushi [Japan Society for the Promotion of Science, Ikenohata1-1-1, Daitou-ku, Tokyo 110-0008 (Japan) and Creative Research Initiative ' Sousei' , Hokkaido University, Sapporo, Hokkaido 001-0021 (Japan)]. E-mail: MATSUDA.Atsushi@nims.go.jp; Ikoma, Toshiyuki [Biomaterials Research Center, National Institute for Materials Science, Namiki 1-1, Tsukuba, Ibaraki 305-0044 (Japan); Kobayashi, Hisatoshi [Biomaterials Research Center, National Institute for Materials Science, Namiki 1-1, Tsukuba, Ibaraki 305-0044 (Japan)]. E-mail: Kobayashi.Hisatoshi@nims.go.jp; Tanaka, Junzo [Creative Research Initiative ' Sousei' , Hokkaido University, Sapporo, Hokkaido 001-0021 (Japan); Biomaterials Research Center, National Institute for Materials Science, Namiki 1-1, Tsukuba, Ibaraki 305-0044 (Japan)

    2004-12-01

    Core-shell type chitosan/calcium phosphate composite fibers were prepared by a facile wet spinning method; the chitosan aqueous solution with PO{sub 4} ions was dropped and coagulated in the ethanol/calcium hydroxide solutions at different mixed ratio. X-ray diffraction (XRD) patterns indicated that the crystal phases of calcium phosphates in the composite fibers were a low-crystalline hydroxyapatite (HAp; Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2})or the low-crystalline hydroxyapatite/brushite mixture depended on the ratio of ethanol/calcium hydroxide solutions. The inorganic contents were ca. 60 wt.% by using the TG-DTA analysis. The energy-dispersive X-ray spectroscopy (EDS) analysis indicated that Ca and P atoms were mainly distributed on the outer layer of the composite fiber to grow calcium phosphate crystals; however, a little amount of P atom still remained at the inside of the fiber. This indicated that the composite fibers formed a unique core-shell structure with shell of calcium phosphate and core of chitosan. The mechanical property of the fibers was reinforced by the initial concentration of chitosan solution.

  10. Magnesium substitution in brushite cements.

    Science.gov (United States)

    Alkhraisat, Mohammad Hamdan; Cabrejos-Azama, Jatsue; Rodríguez, Carmen Rueda; Jerez, Luis Blanco; Cabarcos, Enrique López

    2013-01-01

    The use of magnesium-doped ceramics has been described to modify brushite cements and improve their biological behavior. However, few studies have analyzed the efficiency of this approach to induce magnesium substitution in brushite crystals. Mg-doped ceramics composed of Mg-substituted β-TCP, stanfieldite and/or farringtonite were reacted with primary monocalcium phosphate (MCP) in the presence of water. The cement setting reaction has resulted in the formation of brushite and newberyite within the cement matrix. Interestingly, the combination of SAED and EDX analyses of single crystal has indicated the occurrence of magnesium substitution within brushite crystals. Moreover, the effect of magnesium ions on the structure, and mechanical and setting properties of the new cements was characterized as well as the release of Ca(2+) and Mg(2+) ions. Further research would enhance the efficiency of the system to incorporate larger amounts of magnesium ions within brushite crystals.

  11. Preparation, physical-chemical characterization, and cytocompatibility of polymeric calcium phosphate cements.

    Science.gov (United States)

    Khashaba, Rania M; Moussa, Mervet; Koch, Christopher; Jurgensen, Arthur R; Missimer, David M; Rutherford, Ronny L; Chutkan, Norman B; Borke, James L

    2011-01-01

    Aim. Physicochemical mechanical and in vitro biological properties of novel formulations of polymeric calcium phosphate cements (CPCs) were investigated. Methods. Monocalcium phosphate, calcium oxide, and synthetic hydroxyapatite were combined with either modified polyacrylic acid, light activated polyalkenoic acid, or polymethyl vinyl ether maleic acid to obtain Types I, II, and III CPCs. Setting time, compressive and diametral strength of CPCs was compared with zinc polycarboxylate cement (control). Specimens were characterized using X-ray diffraction, scanning electron microscopy, and infrared spectroscopy. In vitro cytotoxicity of CPCs and control was assessed. Results. X-ray diffraction analysis showed hydroxyapatite, monetite, and brushite. Acid-base reaction was confirmed by the appearance of stretching peaks in IR spectra of set cements. SEM revealed rod-like crystals and platy crystals. Setting time of cements was 5-12 min. Type III showed significantly higher strength values compared to control. Type III yielded high biocompatibility. Conclusions. Type III CPCs show promise for dental applications.

  12. Growth of brushite crystals in sodium silicate gel and their characterization

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, R.R.; Wang, M. [Nanyang Technological Univ. (Singapore). School of Mechanical and Production Engineering

    2001-07-01

    Brushite (CaHPO{sub 4}.2H{sub 2}O, DCPD) single crystals were grown in sodium silicate gel at room temperature. The single diffusion technique was employed in growing crystals. Suitable reactants such as ammonium di-hydrogen phosphate and calcium nitrate tetra hydrate were used as inner and outer reactants. Growth parameters, such as concentration of reactants, gel density and period of growth, were investigated. With 1M ammonium di-hydrogen phosphate and 2M calcium nitrate tetra hydrate, Brushite needles of the size up to 40 mm in length were obtained in a period of 45 days. The crystals grown were confirmed to be Brushite by XRD and FTIR analyses. As determined by nano-indentation tests, these crystals had average modulus and hardness values of 22.5 GPa and 1.75 GPa, respectively. (orig.)

  13. The effect of hyaluronic acid on brushite cement cohesion.

    Science.gov (United States)

    Alkhraisat, M H; Rueda, C; Mariño, F T; Torres, J; Jerez, L B; Gbureck, U; Cabarcos, E L

    2009-10-01

    The improvement of calcium phosphate cement (CPC) cohesion is essential for its application in highly blood perfused regions. This study reports the effectiveness of hyaluronic acids of different molecular weights in the enhancement of brushite cement cohesion. The cement was prepared using a powder phase composed of a mixture of beta-tricalcium phosphate and monocalcium phosphate monohydrate, whereas the liquid phase was formed by 0.5M citric acid solution modified by the addition of hyaluronic acid of different molecular weights. It was found that medium and high molecular weight hyaluronic acid enhances the cement cohesion and scarcely affects the cement mechanical properties. However, concentrations >0.5% (w/v) were less efficient to prevent the cement disintegration. It is concluded that hyaluronic acid could be applied efficiently to reduce brushite cement disintegration.

  14. Apatite Formation from Amorphous Calcium Phosphate and Mixed Amorphous Calcium Phosphate/Amorphous Calcium Carbonate.

    Science.gov (United States)

    Ibsen, Casper J S; Chernyshov, Dmitry; Birkedal, Henrik

    2016-08-22

    Crystallization from amorphous phases is an emerging pathway for making advanced materials. Biology has made use of amorphous precursor phases for eons and used them to produce structures with remarkable properties. Herein, we show how the design of the amorphous phase greatly influences the nanocrystals formed therefrom. We investigate the transformation of mixed amorphous calcium phosphate/amorphous calcium carbonate phases into bone-like nanocrystalline apatite using in situ synchrotron X-ray diffraction and IR spectroscopy. The speciation of phosphate was controlled by pH to favor HPO4 (2-) . In a carbonate free system, the reaction produces anisotropic apatite crystallites with large aspect ratios. The first formed crystallites are highly calcium deficient and hydrogen phosphate rich, consistent with thin octacalcium phosphate (OCP)-like needles. During growth, the crystallites become increasingly stoichiometric, which indicates that the crystallites grow through addition of near-stoichiometric apatite to the OCP-like initial crystals through a process that involves either crystallite fusion/aggregation or Ostwald ripening. The mixed amorphous phases were found to be more stable against phase transformations, hence, the crystallization was inhibited. The resulting crystallites were smaller and less anisotropic. This is rationalized by the idea that a local phosphate-depletion zone formed around the growing crystal until it was surrounded by amorphous calcium carbonate, which stopped the crystallization.

  15. MULTIPLE SCATTERING IN THE EXAFS OF CALCIUM PHOSPHATES

    OpenAIRE

    1986-01-01

    Analysis of the EXAFS spectra of hydroxyapatite, brushite and monetite, recorded above the calcium K edge, requires the inclusion of multiple scattering by phosphorus atoms at 0.37 nm, from calcium. If multiple scattering is not included, some variable parameters acquire physically unreasonable values. Atomic radii never had to be varied by more than 0.01 nm from their values in the accepted crystal structures.

  16. Physical Properties of Acidic Calcium Phosphate Cements

    OpenAIRE

    2014-01-01

    The gold standard for bone replacement today, autologous bone, suffers from several disadvantages, such as the increased risk of infection due to the need for two surgeries. Degradable synthetic materials with properties similar to bone, such as calcium phosphate cements, are a promising alternative. Calcium phosphate cements are suited for a limited amount of applications and improving their physical properties could extend their use into areas previously not considered possible. For example...

  17. Biologically mediated resorption of brushite cement in vitro.

    Science.gov (United States)

    Grover, Liam M; Gbureck, Uwe; Wright, Adrian J; Tremayne, Maryjane; Barralet, Jake E

    2006-04-01

    A new calcium phosphate cement is reported, which sets to form a matrix consisting of brushite, dicalcium pyrophosphate dihydrate and an amorphous phase following the mixture of beta-tricalcium phosphate with an aqueous pyrophosphoric acid solution. This reactant combination set within a clinically relevant time-frame (approximately 10 min) and exhibited a higher compressive strength (25 MPa) than previously reported brushite cements. The in vitro degradation of the beta-tricalcium phosphate-pyrophosphoric acid cement was tested in both phosphate buffered saline and bovine serum. The pyrophosphate ion containing cement reported here was found not to be hydrolysed to form hydroxyapatite in vitro like beta-tricalcium phosphate-orthophosphoric acid solution cements. This finding is significant since the formation of hydroxyapatite by hydrolysis is thought to retard in vivo degradation of brushite cements. When aged in bovine serum, the cement lost considerably more mass than when aged in phosphate buffered saline, indicating that proteins, most likely phosphatase enzymes played an important role in the degradation. As pyrophosphate ions are thought to be the source of orthophosphate ions during bone mineralisation, this new class of bone cement offers a route to new degradable synthetic bone grafting materials.

  18. Solid-state phosphorus-31 nuclear magnetic resonance studies of synthetic solid phases of calcium phosphate: potential models of bone mineral.

    Science.gov (United States)

    Aue, W P; Roufosse, A H; Glimcher, M J; Griffin, R G

    1984-12-04

    Phosphorus-31 NMR spectra have been obtained from a variety of synthetic, solid calcium phosphate mineral phases by magic angle sample spinning. The samples include crystalline hydroxyapatite, two type B carbonatoapatites containing 3.2 and 14.5% CO3(2-), respectively, a hydroxyapatite in which approximately 12% of the phosphate groups are present as HPO4(2-), an amorphous calcium phosphate, monetite, brushite, and octacalcium phosphate. Spectra were observed by the standard Bloch decay and cross-polarization techniques, as well as by a dipolar suppression sequence, in order to distinguish between protonated and unprotonated phosphate moieties. The spectra of the synthetic calcium phosphates provide basic information that is essential for interpreting similar spectra obtained from bone and other calcified tissues.

  19. Influence of polymer addition on the mechanical properties of a premixed calcium phosphate cement.

    Science.gov (United States)

    Engstrand, Johanna; Persson, Cecilia; Engqvist, Håkan

    2013-01-01

    Premixed calcium phosphate cements can reduce handling complications that are associated with the mixing of cements in the operating room. However, to extend the clinical indication of ceramic cements their mechanical properties need to be further improved. The incorporation of a polymeric material with intrinsically high tensile properties could possibly assist in increasing the mechanical properties of calcium phosphate cement. In this study polymer microparticles made from poly(lactid-co-glycolide) plasticised with poly(ethylene glycol) 400 (PLGA/PEG microparticles) were added in amounts of up to 5 wt% to a premixed acidic calcium phosphate cement. The PLGA/PEG microparticles added undergo a shape transformation at 37 °C, which could give a better integration between polymer microparticles and ceramic cement compared with polymer microparticles lacking this property. The results showed that the incorporation of 1.25 wt% PLGA/PEG microparticles increased the compressive strength by approximately 20% up to 15.1 MPa while the diametral tensile strength was kept constant. The incorporation of PLGA/PEG microparticles increased the brushite to monetite ratio after setting compared with pure ceramic cements. In conclusion, small amounts of PLGA/PEG microparticles can be incorporated into premixed acidic calcium phosphate cement and increase their mechanical properties, which could lead to increased future applications.

  20. Influence of polymer addition on the mechanical properties of a premixed calcium phosphate cement

    Science.gov (United States)

    Engstrand, Johanna; Persson, Cecilia; Engqvist, Håkan

    2013-01-01

    Premixed calcium phosphate cements can reduce handling complications that are associated with the mixing of cements in the operating room. However, to extend the clinical indication of ceramic cements their mechanical properties need to be further improved. The incorporation of a polymeric material with intrinsically high tensile properties could possibly assist in increasing the mechanical properties of calcium phosphate cement. In this study polymer microparticles made from poly(lactid-co-glycolide) plasticised with poly(ethylene glycol) 400 (PLGA/PEG microparticles) were added in amounts of up to 5 wt% to a premixed acidic calcium phosphate cement. The PLGA/PEG microparticles added undergo a shape transformation at 37 °C, which could give a better integration between polymer microparticles and ceramic cement compared with polymer microparticles lacking this property. The results showed that the incorporation of 1.25 wt% PLGA/PEG microparticles increased the compressive strength by approximately 20% up to 15.1 MPa while the diametral tensile strength was kept constant. The incorporation of PLGA/PEG microparticles increased the brushite to monetite ratio after setting compared with pure ceramic cements. In conclusion, small amounts of PLGA/PEG microparticles can be incorporated into premixed acidic calcium phosphate cement and increase their mechanical properties, which could lead to increased future applications. PMID:24270588

  1. Smart designing of new hybrid materials based on brushite-alginate and monetite-alginate microspheres: Bio-inspired for sequential nucleation and growth

    OpenAIRE

    2014-01-01

    In this report new hybrid materials based on brushite-alginate and monetite-alginate were prepared by self-assembling alginate chains and phosphate source ions via a gelation process with calcium ions. The alginate served as nanoreactor for nucleation and growth of brushite or/and monetite due to its gelling and swelling properties. The alginate gel framework, the crystalline phase and morphology of formed hybrid biomaterials were shown to be strongly dependent upon the concentration of the p...

  2. Brushite cement additives inhibit attachment to cell culture beads.

    Science.gov (United States)

    Jamshidi, Parastoo; Bridson, Rachel H; Wright, Adrian J; Grover, Liam M

    2013-05-01

    Brushite-forming calcium phosphate cements are of great interest as bone replacement materials because they are resorbable in physiological conditions. Cell-attached culture beads formed from this material could be of great use for cell therapy. Despite a significant amount of work on optimizing the physicochemical properties of these materials, there are very few studies that have evaluated the capacity of the materials to facilitate cell adhesion. In this study, we have formed resorbable calcium phosphate (brushite) culture beads and for the first time we showed that cell attachment to the surface of the brushite cement (BC) could be inhibited by the presence of an intermediate dicalcium phosphate-citrate complex, formed in the cement as a result of using citric acid, a retardant and viscosity modifier used in many cement formulations. The BC beads formed from the mixture of β-TCP/orthophosphoric acid using citric acid did not allow cell attachment without further treatment. Ageing of BC beads in serum-free Dulbecco's Modified Eagle's Medium (DMEM) solution at 37°C for 1 week greatly enhanced the cell adhesion capacity of the material. Scanning electron microscopy, X-ray diffraction (XRD), and confocal Raman microspectrometry indicated the increased capacity for cell adhesion was due to the changes in phase composition of BC. XRD patterns collected before and after ageing in aqueous solution and a high initial mass loss, suggest the formation of a dicalcium phosphate-citrate complex within the matrix. Since compacts formed from brushite powder supported cell attachment, it was hypothesized that the dicalcium phosphate-citrate complex prevented attachment to the cement surface.

  3. Effect of poly(aspartic acid) on calcium phosphate removal from stainless steel tubing under turbulent flow conditions

    Science.gov (United States)

    Littlejohn, Felicia

    Calcium phosphate deposition causes cleaning problems in a number of situations including water treatment, dairy processing, and dental applications. This problem is exacerbated by the limited choices of cleaning chemicals that meet environmental regulations. To promote the development of biodegradable, non-toxic alternatives, this research examines the removal of calcium phosphate deposits consisting of brushite (dicalcium phosphate dihydrate; DCPD) and a mixture of hydroxyapatite (HAP) and DCPD from stainless steel in the presence of poly(aspartic acid) and its sodium salt (PASP). The effects of solvent pH, PASP concentration, and flow rate on the calcium phosphate removal rates are measured from stainless steel tubing under turbulent flow conditions using a solid scintillation detection technique. A mechanistic evaluation of the cleaning data in the absence of PASP indicates that DCPD removal is dominated by shear while HAP/DCPD deposit removal is limited by a combination of mass transfer and interfacial processes. Although the removal mechanisms differ, the results conclusively show that PASP promotes calcium phosphate removal under conditions that favor calcium sequestration in both cases. An in-depth study of DCPD removal in the presence of PASP reveals that this additive is most effective under conditions where calcium sequestration and phosphate protonation occur simultaneously.

  4. Thermal stability of the 'cave' mineral brushite CaHPO{sub 4}.2H{sub 2}O - Mechanism of formation and decomposition

    Energy Technology Data Exchange (ETDEWEB)

    Frost, Ray L., E-mail: r.frost@qut.edu.au [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George St., GPO Box 2434, Brisbane, Queensland 4001 (Australia); Palmer, Sara J. [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George St., GPO Box 2434, Brisbane, Queensland 4001 (Australia)

    2011-07-10

    Highlights: {yields} In this study the thermal stability of brushite is reported. {yields} Such a study is relevant to the elimination of renal canal stones. {yields} A mechanism for the formation of brushite is proposed. {yields} A mechanism for the decomposition of brushite is discussed. {yields} This research has implications for the control and removal of kidney stones. - Abstract: Thermogravimetry combined with evolved gas mass spectrometry has been used to ascertain the stability of the 'cave' mineral brushite. X-ray diffraction shows that brushite from the Jenolan Caves is very pure. Thermogravimetric analysis coupled with ion current mass spectrometry shows a mass loss at 111 {sup o}C due to loss of water of hydration. A further decomposition step occurs at 190 {sup o}C with the conversion of hydrogen phosphate to a mixture of calcium ortho-phosphate and calcium pyrophosphate. TG-DTG shows the mineral is not stable above 111 {sup o}C. A mechanism for the formation of brushite on calcite surfaces is proposed, and this mechanism has relevance to the formation of brushite in urinary tracts.

  5. Mechanisms for the removal of calcium phosphate deposits in turbulent flow

    Energy Technology Data Exchange (ETDEWEB)

    Littlejohn, F.; Grant, C.S.; Saez, A.E.

    2000-04-01

    This work investigates the mechanisms for the removal of calcium phosphate deposits from stainless steel tubing in turbulent flows. Two types of deposits were analyzed: brushite (dicalcium phosphate dihydrate, DCPD) and a mixture of DCPD/hydroxyapatite (HAP). Cleaning studies were carried out at pHs ranging from 2.85 to 10. The data were analyzed by means of a mathematical model that incorporates the effects of interfacial dissolution and mass transfer. The results show that the HAP/DCPD cleaning rate is influenced both by the kinetics of the interfacial dissolution and by mass transfer. Within the same range of experimental conditions, the rate-limiting mechanism for DCPD removal was the abrasion of the solid by shear stresses. In this case, the interfacial dissolution process plays the role of decreasing the structural integrity of the deposit. These findings show that the removal mechanism of the HAP/DCPD mixture differs significantly from the behavior of individual components.

  6. The porosity and roughness of electrodeposited calcium phosphate coatings in simulated body fluid

    Directory of Open Access Journals (Sweden)

    Đošić Marija S.

    2015-01-01

    Full Text Available Calcium phosphate coatings were electrochemically deposited on titanium from the aqueous solution of Ca(NO32 and NH4H2PO4 with the current density of 10 mA cm-2 for deposition time of 15 min. The obtained brushite coatings, (CaHPO4·2H2O, were converted to hydroxyapatite (HA by soaking in simulated body fluid (SBF for 2, 7 and 14 days. The brushite and hydroxyapatite coatings were characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM and atomic force microscopy (AFM. It was shown that the increase in soaking time increases the porosity, roughness and crystallite domain size of HA coatings and decreases the unit cell parameters and unit cell volume, while does not affect the HA mean pore area. The calcium and phosphorus ions concentrations in SBF were determined by atomic absorption spectroscopy (AAS and UV-Vis spectroscopy, respectively and the mechanism of HA growth based on dissolution-precipitation was proposed. [Projekat Ministarstva nauke Republike Srbije, br. III 45019, br. III 45015 i br. OI 72004

  7. The fabrication of nanocomposites via calcium phosphate formation on gelatin-chitosan network and the gelatin influence on the properties of biphasic composites

    Energy Technology Data Exchange (ETDEWEB)

    Babaei, Zahra [Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol (Iran, Islamic Republic of); Jahanshahi, Mohsen, E-mail: mjahan@nit.ac.ir [Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol (Iran, Islamic Republic of); Rabiee, Sayed Mahmood [Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol (Iran, Islamic Republic of); School of Mechanical Engineering, Babol University of Technology, Babol (Iran, Islamic Republic of)

    2013-01-01

    A novel biodegradable polymer-ceramic nanocomposite which consisted of gelatin (Gel), chitosan (CS), and calcium phosphate (CaP) nanoparticles was prepared based on in situ preparation method. The fabricated biocomposites were characterized by FTIR, X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscope with X-ray elemental analysis (SEM-EDX). The characterization results confirmed that the crystalline calcium phosphate nanoparticles were mineralized in polymeric matrix and the interaction between Ca2+ in calcium phosphate and functional groups in polymers molecular chains was formed. XRD result showed that in addition to hydroxyapatite (HA), Brushite (BR) and tricalcium phosphate ({beta}-TCP) particles also were formed due to lack of complete penetration of the basic solution into the polymeric matrix. However, SEM image indicated that the polymeric matrix has the controlling role in the particle size of calcium phosphate. The size of particles in three component composites was about 100 nm while in two component composites proved to be more in {mu}m size. TEM observation supported SEM results and showed that the three component composites have calcium phosphate nanoparticles. The elastic modulus and compressive strength of the composites were also improved by the employment of gelatin and chitosan together, which can make them more beneficial for surgical applications. - Highlights: Black-Right-Pointing-Pointer A new type of calcium phosphate nanocomposites consisted chitosan and gelatin as polymeric matrix was obtained via in situ precipitation method. Black-Right-Pointing-Pointer The formed particles into the polymeric matrix are hydroxyapatite, Brushite and {beta}-tricalcium phosphate. Black-Right-Pointing-Pointer The polymer concentration is a predominant factor for inhibiting nucleation and growth of calcium phosphate particles as the particles size was also decreased by increasing the amount of polymeric

  8. Biomimetic synthesis of poly(propylene-fumarate)-calcium phosphate composites for tissue engineering

    Science.gov (United States)

    Hakimi Mehr, Dorna

    A novel in-situ co-precipitation process for the synthesis of poly(propylene-fumarate)-calcium phosphate composites was developed. In this process the calcium phosphate phase nucleates and grows in the presence of poly(propylene-fumarate) (PPF), in a novel two-solvent system including tetrahydrofuran (THF) and water. It was found that the presence of the organic solvent (THF) does not affect the phase evolution of the calcium phosphate. Both in the presence and absence of THF crystalline dicalcium phosphate dihydrate (DCPD, brushite) and poorly crystalline hydroxyapatite (HAp) form, and transform to crystalline HAp after 24 hours of synthesis time. Contrary to the organic solvent, PPF has a significant influence on the calcium phosphate phase that forms in its presence. It is found that PPF provides a template for the formation of the calcium phosphate phase through a coordination bond between the calcium ion and the carbonyl group of the polymer. As a result of this templating, hydroxyapatite can form in a significantly shorter period of time (˜1 hr) compared to the system where PPF is not present (24 hrs). The nature of the calcium phosphate phase that forms in the presence of PPF depends on the molecular weight and concentration of PPF. High concentration of PPF in the composite (e.g. 80%) stabilizes an amorphous calcium phosphate (ACP) phase and hinders its transformation to crystalline apatite, while low concentration of PPF (e.g. 5%) promotes the formation of crystalline apatite. Higher molecular weight PPF (Mw = 4500) is found to be more efficient in stabilizing the amorphous phase compared to lower molecular weight PPF (Mw = 1800). While high molecular weight PPF stabilizes ACP, low molecular weight PPF promotes its conversion to crystalline apatite. TEM observations revealed that flake-like hydroxyapatite crystals form in the absence of PPF while spherical ACP particles form in a composite containing 80% PPF. The ACP nano-particles (50-100 nm in diameter

  9. Smart designing of new hybrid materials based on brushite-alginate and monetite-alginate microspheres: Bio-inspired for sequential nucleation and growth

    Energy Technology Data Exchange (ETDEWEB)

    Amer, Walid [MAScIR Foundation, INANOTECH, Rabat Design, Rue Mohamed El Jazouli, Madinat El Irfane 10100 Rabat (Morocco); Abdelouahdi, Karima [Centre National pour la Recherche Scientifique et Technique (CNRST), Division UATRS, Angle Allal Fassi/FAR, B.P. 8027, Hay Riad, 10000 Rabat (Morocco); Ramananarivo, Hugo Ronald; Fihri, Aziz; El Achaby, Mounir [MAScIR Foundation, INANOTECH, Rabat Design, Rue Mohamed El Jazouli, Madinat El Irfane 10100 Rabat (Morocco); Zahouily, Mohamed [Laboratoire de Matériaux, Catalyse et Valorisation des Ressources Naturelles, URAC 24, Faculté des Sciences et Techniques, Université Hassan II, Mohammedia B.P. 146, 20650 (Morocco); Barakat, Abdellatif [SUPAGRO-INRA-CIRAD-UMR IATE 1208, Ingenierie des Agropolymères et Technologies Emergentes, 2, Place Pierre Viala-Bât 31, 34060 Montpellier cedex 1 (France); Djessas, Kamal [CNRS-PROMES Tecnosud, F-66100 Perpignan (France); Clark, James [Green Chemistry, Centre of Excellence, University of York, York YO10 5DD (United Kingdom); Solhy, Abderrahim, E-mail: a.solhy@mascir.com [MAScIR Foundation, INANOTECH, Rabat Design, Rue Mohamed El Jazouli, Madinat El Irfane 10100 Rabat (Morocco)

    2014-02-01

    In this report new hybrid materials based on brushite-alginate and monetite-alginate were prepared by self-assembling alginate chains and phosphate source ions via a gelation process with calcium ions. The alginate served as nanoreactor for nucleation and growth of brushite or/and monetite due to its gelling and swelling properties. The alginate gel framework, the crystalline phase and morphology of formed hybrid biomaterials were shown to be strongly dependent upon the concentration of the phosphate precursors. These materials were characterized by thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray analysis (EDX). - Graphical abstract: A new class of hybrid materials based on brushite{sub a}lginate and monetite{sub a}lginate were prepared for the first time by adopting a soft and clean route. Thanks to their gelling and swelling properties, alginate porous polysaccharide microspheres behave as nanoreactors for nucleating, growing and hosting of the phosphate cements such as brushite or monetite. - Highlights: • New structured hybrid materials are prepared from biopolymer and phosphates. • Evidence for a new route for the synthesis of hybrid materials alginate-brushite and alginate-monetite via ionotropic gel of alginate. • The concentration of phosphate has a role crucial for selectivity to monetite or brushite.

  10. Protein content of human apatite and brushite kidney stones: significant correlation with morphologic measures.

    Science.gov (United States)

    Pramanik, Rocky; Asplin, John R; Jackson, Molly E; Williams, James C

    2008-10-01

    Apatite and brushite kidney stones share calcium and phosphate as their main inorganic components. We tested the hypothesis that these stone types differ in the amount of proteins present in the stones. Intact stones were intensively analyzed by microcomputed tomography (micro CT) for both morphology (including the volume of voids, i.e., space devoid of X-ray dense material) and mineral type. To extract all proteins present in kidney stones in soluble form we developed a three-step extraction procedure using the ground stone powder. Apatite stones had significantly higher levels of total protein content and void volume compared to brushite stones. The void volume was highly correlated with the total protein contents in all stones (r2 = 0.61, P brushite stones contained significantly fewer void regions and proteins than did apatite stones (3.2 +/- 4.5% voids for brushite vs. 10.8 +/- 11.2% for apatite, P brushite vs. 6.0 +/- 2.4% for apatite, P brushite and apatite stones is higher than that was previously thought, and also suggest that micro CT-visible void regions are related to the presence of protein.

  11. Three-dimensionally Perforated Calcium Phosphate Ceramics

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Porous calcium phosphate ceramics were produced by compression molding using a special mold followed by sintering. The porous calcium phosphate ceramics have three-dimensional and penetrated open pores380-400μm in diameter spaced at intervals of 200μm. The layers of the linear penetration pores alternately lay perpendicular to pore direction. The porosity was 59%-65% . The Ca/P molar ratios of the porous calcium phosphate ceramics range from 1.5 to 1.85. A binder containing methyl cellulose was most effective for preparing the powder compact among vinyl acetate, polyvinyl alcohol, starch, stearic acid, methyl cellulose and their mixtures. Stainless steel, polystyrene, nylon and bamboo were used as the long columnar male dies for the penetrated open pores. When polystyrene, nylon and bamboo were used as the long columnar male dies, the dies were burned out during the sintering process. Using stainless steel as the male dies with the removal of the dies before heat treatment resulted in a higher level of densification of the calcium phosphate ceramic.

  12. Electrosprayed calcium phosphate coatings for biomedical purposes

    NARCIS (Netherlands)

    Leeuwenburgh, Sander Cornelis Gerardus

    2006-01-01

    In this thesis, the suitability of the Electrostatic Spray Deposition (ESD) technique was studied for biomedical purposes, i.e., deposition of calcium phosphate (CaP) coatings onto titanium substrates. Using ESD, which is a simple and cheap deposition method for inorganic and organic coatings, it wa

  13. Low temperature fabrication of spherical brushite granules by cement paste emulsion.

    Science.gov (United States)

    Moseke, Claus; Bayer, Christoph; Vorndran, Elke; Barralet, Jake E; Groll, Jürgen; Gbureck, Uwe

    2012-11-01

    Secondary protonated calcium phosphates such as brushite (CaHPO(4)·2H(2)O) or monetite (CaHPO(4)) have a higher resorption potential in bone defects than sintered ceramics, e.g. tricalcium phosphate or hydroxyapatite. However, processing of these phosphates to monolithic blocks or granules is not possible by sintering due to thermal decomposition of protonated phosphates at higher temperatures. In this study a low temperature technique for the preparation of spherical brushite granules in a cement setting reaction is presented. These granules were synthesized by dispersing a calcium phosphate cement paste composed of β-tricalcium phosphate and monocalcium phosphate together with a surfactant to an oil/water emulsion. The reaction products were characterized regarding their size distribution, morphology, and phase composition. Clinically relevant granule sizes ranging from 200 μm to 1 mm were obtained, whereas generally smaller granules were received with higher oil viscosity, increasing temperature or higher powder to liquid ratios of the cement paste. The hardened granules were microporous with a specific surface area of 0.7 m(2)/g and consisted of plate-like brushite (>95 % according to XRD) crystals of 0.5-7 μm size. Furthermore it was shown that the granules may be also used for drug delivery applications. This was demonstrated by adsorption of vancomycin from an aqueous solution, where a load of 1.45-1.88 mg drug per g granules and an almost complete release within 2 h was obtained.

  14. Preparation and characterization of calcium phosphate biomaterials.

    Science.gov (United States)

    Calafiori, A R; Di Marco, G; Martino, G; Marotta, M

    2007-12-01

    Calcium phosphate cement (CPC) samples have been prepared with a mixture of monocalciumphosphate monohydrate (MCPM) and calcium carbonate (CC) powders, in stechiometric moles ratio 1:2.5 to obtain a Ca/P ratio of about 1.67 typical of hydroxyapatite (HAp), with or without addition of HAp. All specimens are incubated at 30 degrees C in a steam saturated air environment for 3, 6 and 15 days respectively, afterwards dried and stored under nitrogen. The calcium phosphate samples have been characterized by X-ray diffraction (XRD), Vickers hardness test (HV), diametral compression (d.c.), strength compression, and porosity evaluation. MCPM/CC mixture has a 30% HAp final concentration and is characterized by higher porosity (amount 78%) and mechanical properties useful as filler in bone segments without high mechanical stress.

  15. 21 CFR 582.6215 - Monobasic calcium phosphate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Monobasic calcium phosphate. 582.6215 Section 582.6215 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED....6215 Monobasic calcium phosphate. (a) Product. Monobasic calcium phosphate. (b) Conditions of use....

  16. 21 CFR 182.6215 - Monobasic calcium phosphate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Monobasic calcium phosphate. 182.6215 Section 182.6215 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED....6215 Monobasic calcium phosphate. (a) Product. Monobasic calcium phosphate. (b) Conditions of use....

  17. Osteoclastic resorption of biomimetic calcium phosphate coatings in vitro.

    NARCIS (Netherlands)

    Leeuwenburgh, S.C.G.; Layrolle, P.; Barrere, F.; Bruijn, J.G.M. de; Schoonman, J.; Blitterswijk, C.A. van; Groot, K. de

    2001-01-01

    A new biomimetic method for coating metal implants enables the fast formation of dense and homogeneous calcium phosphate coatings. Titanium alloy (Ti6Al4V) disks were coated with a thin, carbonated, amorphous calcium phosphate (ACP) by immersion in a saturated solution of calcium, phosphate, magnesi

  18. RAPID ASSOCIATION OF UNCONJUGATED BILIRUBIN WITH AMORPHOUS CALCIUM-PHOSPHATE

    NARCIS (Netherlands)

    VANDERVEERE, CN; SHOEMAKER, B; VANDERMEER, R; GROEN, AK; JANSEN, PLM; ELFERINK, RPJO

    1995-01-01

    The association of unconjugated bilirubin (UCB) with amorphous calcium phosphate was studied in vitro. To this end UCB, solubilized in different micellar bile salt solutions, was incubated with freshly prepared calcium phosphate precipitate. It was demonstrated that amorphous calcium phosphate (ACP)

  19. Transfection system of amino-functionalized calcium phosphate nanoparticles: in vitro efficacy, biodegradability, and immunogenicity study.

    Science.gov (United States)

    Mostaghaci, Babak; Susewind, Julia; Kickelbick, Guido; Lehr, Claus-Michael; Loretz, Brigitta

    2015-03-11

    Many methods have been developed in order to use calcium phosphate (CaP) for delivering nucleotides into living cells. Surface functionalization of CaP nanoparticles (CaP NPs) with N-(2-aminoethyl)-3-aminopropyltrimethoxysilane was shown recently to achieve dispersed NPs with a positive surface charge, capable of transfection (Chem. Mater. 2013, 25 (18), 3667). In this study, different crystal structures of amino-modified CaP NPs (brushite and hydroxyapatite) were investigated for their interaction in cell culture systems in more detail. Qualitative (confocal laser scanning microscopy) and quantitative (flow cytometry) transfection experiments with two cell lines showed the higher transfection efficacy of brushite versus hydroxyapatite. The transfection also revealed a cell type dependency. HEK293 cells were easier to transfect compared to A549 cells. This result was supported by the cytotoxicity results. A549 cells showed a higher degree of tolerance toward the CaP NPs. Further, the impact of the surface modification on the interaction with macrophages and complement as two important components of the innate immune system were considered. The amine surface functionalization had an effect of decreasing the release of proinflammatory cytokines. The complement interaction investigated by a C3a complement activation assay did show no significant differences between CaP NPs without or with amine modification and overall weak interaction. Finally, the degradation of CaP NPs in biological media was studied with respect to the two crystal structures and at acidic and neutral pH. Both amino-modified CaP NPs disintegrate within days at neutral pH, with a notable faster disintegration of brushite NPs at acidic pH. In summary, the fair transfection capability of this amino functionalized CaP NPs together with the excellent biocompatibility, biodegradability, and low immunogenicity make them interesting candidates for further evaluation.

  20. X-Ray Diffraction Technique in the Analysis of Phases of Hydroxylapatite and Calcium Phosphate in a Human Jaw

    Directory of Open Access Journals (Sweden)

    Srđan D. Poštić

    2014-06-01

    Full Text Available Objective: Human jawbones consist mainly of hydroxylapatite. The aim of this study was to assess the structure of solid calcium phosphate compounds of the jawbone in cases of normal and osteoporotic JBs. Design: The X-ray diffraction technique was used to analyze the structure of samples of cadavers’ jawbones. The experimental JB samples were taken from an osteoporotic and atrophic jawbone, and control samples were from normal and nonosteoporotic bone samples. Results: Hydroxylapatite was the only phase in control bone samples. In experimental bone samples, the above-mentioned phase was registered, as well as monetite and brushite. Conclusion: The obtained data indicated that the changes of crystalographic forms of calcium phosphate in the physiologic system were balanced according to the possibility of change in the inorganic chemical system.

  1. The final phases of calcium and magnesium phosphates precipitated from solutions of high to medium concentration

    Science.gov (United States)

    Abbona, Francesco; Lundager Madsen, Hans Erik; Boistelle, Roland

    1988-07-01

    The phases of calcium and magnesium phosphates, which are obtained by evolution at 25°C of the first precipitates in their mother solutions, are described in terms of pH and composition of solutions. The initial conditions were: 0.050M ≤ [P] ≤ 0.500M; [P] = [Ca] + [Mg]; 0 ≤ [Mg]/[Ca] ≤ 1. The most abundant final phases are brushite, CaHPO 4·2H 2O; monetite, CaHPO 4; newberyite, MgHPO 4·3H 2O and struvite, MgNH 4PO 4·6H 2O. At low concentration whitlockite, Ca 9MgH(PO 4) 7, occurs with the amorphous phase previously precipitated, Ca 3(PO 4) 2·nH 2O. The conditions for stability are discussed and the changes observed are interpreted.

  2. Characterization of calcium phosphate powders originating from Phyllacanthus imperialis and Trochidae Infundibulum concavus marine shells.

    Science.gov (United States)

    Tămăşan, M; Ozyegin, L S; Oktar, F N; Simon, V

    2013-07-01

    The study reports the preparation and characterization of powders consisting of the different phases of calcium phosphates that were obtained from the naturally derived raw materials of sea-shell origins reacted with H3PO4. Species of sea origin, such as corals and nacres, attracted a special interest in bone tissue engineering area. Nacre shells are built up of calcium carbonate in aragonite form crystallized in an organic matrix. In this work two natural marine origin materials (shells of echinoderm Sputnik sea urchin - Phyllacanthus imperialis and Trochidae Infundibulum concavus mollusk) were involved in the developing powders of calcium phosphate based biomaterials (as raw materials for bone-scaffolds) by hotplate and ultrasound methods. Thermal analyses of the as-prepared materials were made for an assessment of the thermal behavior and heat treatment temperatures. Samples from both sea shells each of them prepared by the above mentioned methods were subjected to thermal treatments at 450 °C and 850 °C in order to evaluate the crystalline transformations of the calcium phosphate structures in the heating process. By X-ray diffraction analyses various calcium phosphate phases were identified. In Sputnik sea urchins originated samples were found predominantly brushite and calcite as a small secondary phase, while in Trochidae I. concavus samples mainly monetite and HA phases were identified. Thermal treatment at 850 °C resulted flat-plate whitlockite crystals - β-MgTCP [(Ca, Mg)3 (PO4)2] for both samples regardless the preparation method (ultrasound or hotplate) or the targeted Ca/P molar ratio according with XRD patterns. Scanning electron microscopy and Fourier transformed infrared spectroscopy were involved more in the characterization of these materials and the good correlations of the results of these methods were made.

  3. Characterization of calcium phosphate powders originating from Phyllacanthus imperialis and Trochidae Infundibulum concavus marine shells

    Energy Technology Data Exchange (ETDEWEB)

    Tămăşan, M., E-mail: monica.tamasan@phys.ubbcluj.ro [Babeş-Bolyai University, Faculty of Physics and Interdisciplinary Research Institute on Bio-Nano-Sciences, Cluj-Napoca (Romania); Ozyegin, L.S. [Marmara University, Istanbul (Turkey); Oktar, F.N. [Marmara University, Faculty of Engineering, Department of Bioengineering, Göztepe Campus, Kadıköy 34722, Istanbul (Turkey); Marmara University, School of Health Related Professions, Department of Medical Imaging Technics, Haydarpaşa Campus, Tıbbiye Street, 49, Üsküdar 34668, Istanbul (Turkey); Marmara University, Nanotechnology and Biomaterials Application and Research Centre, Göztepe Campus, Kadıköy 34722, Istanbul (Turkey); Simon, V. [Babeş-Bolyai University, Faculty of Physics and Interdisciplinary Research Institute on Bio-Nano-Sciences, Cluj-Napoca (Romania)

    2013-07-01

    The study reports the preparation and characterization of powders consisting of the different phases of calcium phosphates that were obtained from the naturally derived raw materials of sea-shell origins reacted with H{sub 3}PO{sub 4}. Species of sea origin, such as corals and nacres, attracted a special interest in bone tissue engineering area. Nacre shells are built up of calcium carbonate in aragonite form crystallized in an organic matrix. In this work two natural marine origin materials (shells of echinoderm Sputnik sea urchin — Phyllacanthus imperialis and Trochidae Infundibulum concavus mollusk) were involved in the developing powders of calcium phosphate based biomaterials (as raw materials for bone-scaffolds) by hotplate and ultrasound methods. Thermal analyses of the as-prepared materials were made for an assessment of the thermal behavior and heat treatment temperatures. Samples from both sea shells each of them prepared by the above mentioned methods were subjected to thermal treatments at 450 °C and 850 °C in order to evaluate the crystalline transformations of the calcium phosphate structures in the heating process. By X-ray diffraction analyses various calcium phosphate phases were identified. In Sputnik sea urchins originated samples were found predominantly brushite and calcite as a small secondary phase, while in Trochidae I. concavus samples mainly monetite and HA phases were identified. Thermal treatment at 850 °C resulted flat-plate whitlockite crystals — β-MgTCP [(Ca, Mg){sub 3} (PO{sub 4}){sub 2}] for both samples regardless the preparation method (ultrasound or hotplate) or the targeted Ca/P molar ratio according with XRD patterns. Scanning electron microscopy and Fourier transformed infrared spectroscopy were involved more in the characterization of these materials and the good correlations of the results of these methods were made. - Highlights: ► Calcium phosphate powders are obtained from the crushed shells of 2

  4. Doxycycline sustained release from brushite cements for the treatment of periodontal diseases.

    Science.gov (United States)

    Tamimi, Faleh; Torres, Jesús; Bettini, Ruggero; Ruggera, Francesca; Rueda, Carmen; López-Ponce, Manuel; Lopez-Cabarcos, Enrique

    2008-06-01

    Doxycycline (DOXY) is a wide spectrum antibiotic used in the treatment of dental, periodontal, and bone infections. Brushite cements are calcium phosphate biomaterials especially interesting for bone regeneration processes. In this work, we describe the preparation of a brushite cement containing DOXY and the drug release from the cement. DOXY solutions were mixed with the cement powder and after a 50% burst release in the first 12 h, a slow and controlled release was achieved over 3.5 days. The release of DOXY hyclate was controlled by both, diffusion and Ca(2+) interaction. Formation of DOXY-Ca(2+) chelates was detected in the cement structure using solid state fluorescence. The brushite cement loaded with DOXY hyclate had antibacterial activity against periodontal pathogens: Actinobacillus actinomycetemcomitans, Porphyromonas gingivalis, and Bacteroides frosthytus. This new biomaterial may be helpful for the treatment of periodontal diseases.

  5. Solid-liquid adsorption of calcium phosphate on TiO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Chusuei, C.C.; Goodman, D.W.; Stipdonk, M.J. van; Justes, D.R.; Loh, K.H.; Schweikert, E.A.

    1999-10-12

    Calcium phosphate (CP) in aqueous solution was exposed to thin-film TiO{sub 2} surfaces at predetermined times ranging from 10 min to 20 h using a liquid reaction apparatus (LRA). Surface analysis was then performed using X-ray photoelectron (XPS) and Auger electron (AES) spectroscopies and time-of-flight secondary ion mass spectromemtry (ToF-SIMS) with polyatomic primary ions. XPS revealed that CP nucleated and grew on the TiO{sub 2} surface, with phosphate groups growing on top of an initial 2-dimensional (2D) Ca-rich layer. AES depth profiling of a 4-h solution exposure complemented this finding and gave additional evidence for 3-dimensional (3D) phosphate islands forming on top of the calcium. ToF-SIMS analysis of CP adsorbed on the surface indicated that the predominant phase on the surface was brushite, CaHPO{sub 4}{sm{underscore}bullet}2H{sub 2}O. A model for Ca{sup 2+} cation bridging at the oxide interface is proposed.

  6. Synthesis of the refined calcium phosphate for bone china porcelain from oyster shell

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Y.H. [Department of Environmental Engineering, Kumsung Environment College (Korea, Republic of); Chang, Pok-Ki; Lim, Yong-Mu [Department of Inorganic Materials Engineering, Chonnam National University, Kwangju (Korea, Republic of)

    1997-11-01

    In this study, the oyster shell was calcined at high temperature (>800 deg. C) in reducing atmosphere to remove impurities, refined by elutriation and magnetic separator and reacted with phosphate to synthesized di-calcium phosphate(DCP). Studies for characteristic and application to bone china porcelain of this synthesized DCP were done. By thermal and ICP analysis, the oyster shell was composed of the calcium carbonate(CaCO{sub 3}) with impurities less than 2 wt%. Fe{sub 2}O{sub 3}, TiO{sub 2} and MnO belonged to colouring material and its contents were 0.17, 0.04 and 0.02 wt%, respectively. To research reducing behavior of colouring materials Fe{sub 2}/O{sub 3} was calcined at various temperature in reducing atmosphere. Metal Fe content increased with increasing calcining temperature. After pass through magnetic separator, contents of colouring material were reduced Fe{sub 2}O{sub 3} to 0.07, TiO{sub 2} to 0.03 and MnO to 0.01 wt%, respectively. Di-calcium phosphate synthesized from calcium-hydroxide based upon oyster shell and phosphate in ph=3.5 showed crystalline phase of brushite type, and changed to {Upsilon}-Ca{sub 2}P{sub 2}O{sub 7} at 450 deg. C. For DCP calcined at 1200.deg. C, average particle size was 3.56{mu}m, specific surface area was 1.6851 m{sup 2}/g and had no agglomerate. For bone china used the synthesized DCP, the high temperature slump was 7.5 mm, the shrinkage was 13.7% and the whiteness was 95.26% similarly situated with that of H company. (author). 18 refs., 9 figs., 4 tabs.

  7. Formation of calcium phosphates by vapour diffusion in highly concentrated ionic micro-droplets

    Energy Technology Data Exchange (ETDEWEB)

    Iafisco, M. [Alma Mater Studiorum Universita di Bologna, Dipartimento di Chimica ' ' G. Ciamician' ' , Via Selmi 2, 40126 Bologna (Italy); Universita del Piemonte Orientale, Dipartimento di Scienze Mediche, Via Solaroli 4, 28100 Novara (Italy); Delgado-Lopez, J.M.; Gomez-Morales, J.; Hernandez-Hernandez, M.A.; Rodriguez-Ruiz, I. [Laboratorio de Estudios Cristalograficos, IACT CSIC-UGR, Edificio Lopez Neyra, Avenida del Conocimiento, s/n 18100 Armilla (Spain); Roveri, N. [Alma Mater Studiorum Universita di Bologna, Dipartimento di Chimica ' ' G. Ciamician' ' , Via Selmi 2, 40126 Bologna (Italy)

    2011-08-15

    In this work we have used the sitting drop vapour diffusion technique, employing the ''crystallization mushroom '' to analyze the evolution of calcium phosphate crystallization in micro-droplets containing high initial concentrations of Ca{sup 2+} and HPO{sub 4}{sup 2-}. The decomposition of NH{sub 4}HCO{sub 3} solution produces vapours of NH{sub 3} and CO{sub 2} which diffuse through the droplets containing an aqueous solution of Ca(CH{sub 3}COO){sub 2} and (NH{sub 4}){sub 2}HPO{sub 4}. The result is the increase of pH by means of the diffusion of NH{sub 3} gas and the doping of the calcium phosphate with CO{sub 3}{sup 2-} ions by means of the diffusion of CO{sub 2} gas. The pH of the crystallization process is monitored and the precipitates at different times are characterized by XRD, FTIR, TGA, SEM and TEM techniques. The slow increase of pH and the high concentration of Ca{sup 2+} and HPO{sub 4}{sup 2-} in the droplets induce the crystallization of three calcium phosphate phases: dicalcium phosphate dihydrate (DCPD, brushite), octacalcium phosphate (OCP) and carbonate-hydroxyapatite (HA). The amount of HA nanocrystals with needle-like morphology and dimensions of about 100 nm, closely resembling the inorganic phase of bones, gradually increases, with the precipitation time up to 7 days, whereas the amount of DCPD, growing along the b axis, increases up to 3 days. Then, DCDP crystals start to hydrolyze yielding OCP nanoribbons and HA nanocrystals. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  8. Controlled mineralisation and recrystallisation of brushite within alginate hydrogels.

    Science.gov (United States)

    Bjørnøy, Sindre H; Bassett, David C; Ucar, Seniz; Andreassen, Jens-Petter; Sikorski, Pawel

    2016-02-02

    Due to high solubility and fast resorption behaviour under physiological conditions, brushite (CaHPO4⋅2H2O, calcium monohydrogen phosphate dihydrate, dicalcium phosphate dihydrate) has great potential in bone regeneration applications, both in combination with scaffolds or as a component of calcium phosphate cements. The use of brushite in combination with hydrogels opens up possibilities for new cell-based tissue engineering applications of this promising material. However, published preparation methods of brushite composites, in which the mineral phase is precipitated within the hydrogel network, fail to offer the necessary degree of control over the mineral phase, content and distribution within the hydrogel matrix. The main focus of this study is to address these shortcomings by determining the precise fabrication parameters needed to prepare composites with controlled composition and properties. Composite alginate microbeads were prepared using a counter-diffusion technique, which allows for the simultaneous crosslinking of the hydrogel and precipitation of an inorganic mineral phase. Reliable nucleation of a desired mineral phase within the alginate network proved more challenging than simple aqueous precipitation. This was largely due to ion transport within the hydrogel producing concentration gradients that modified levels of supersaturation and favoured the nucleation of other phases such as hydroxyapatite and octacalcium phosphate, which would otherwise not form. To overcome this, the incorporation of brushite seed crystals resulted in good control during the mineral phase, and by adjusting the number of seeds and amount of precursor concentration, the amount of mineral could be tuned. The material was characterised with a range of physical techniques, including scanning electron microscopy, powder x-ray diffraction and Rietveld refinement, Fourier transform infrared spectroscopy, and thermogravimetric analysis, in order to assess the mineral

  9. Monetite and brushite coated magnesium: in vivo and in vitro models for degradation analysis.

    Science.gov (United States)

    Shadanbaz, Shaylin; Walker, Jemimah; Woodfield, Tim B F; Staiger, Mark P; Dias, George J

    2014-01-01

    The use of magnesium (Mg) as a biodegradable metallic replacement of permanent orthopaedic materials is a current topic of interest and investigation. The appropriate biocompatibility, elastic modulus and mechanical properties of Mg recommend its suitability for bone fracture fixation. However, the degradation rates of Mg can be rapid and unpredictable resulting in mass hydrogen production and potential loss of mechanical integrity. Thus the application of calcium phosphate coatings has been considered as a means of improving the degradation properties of Mg. Brushite and monetite are utilized and their degradation properties (alongside uncoated Mg controls) are assessed in an in vivo subcutaneous environment and the findings compared to their in vitro degradation behaviour in immersion tests. The current findings suggest monetite coatings have significant degradation protective effects compared to brushite coatings in vivo. Furthermore, it is postulated that an in vitro immersion test may be used as a tentative predictor of in vivo subcutaneous degradation behavior of calcium phosphate coated and uncoated Mg.

  10. Smart designing of new hybrid materials based on brushite-alginate and monetite-alginate microspheres: bio-inspired for sequential nucleation and growth.

    Science.gov (United States)

    Amer, Walid; Abdelouahdi, Karima; Ramananarivo, Hugo Ronald; Fihri, Aziz; El Achaby, Mounir; Zahouily, Mohamed; Barakat, Abdellatif; Djessas, Kamal; Clark, James; Solhy, Abderrahim

    2014-02-01

    In this report new hybrid materials based on brushite-alginate and monetite-alginate were prepared by self-assembling alginate chains and phosphate source ions via a gelation process with calcium ions. The alginate served as nanoreactor for nucleation and growth of brushite or/and monetite due to its gelling and swelling properties. The alginate gel framework, the crystalline phase and morphology of formed hybrid biomaterials were shown to be strongly dependent upon the concentration of the phosphate precursors. These materials were characterized by thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray analysis (EDX).

  11. Electrochemical characteristics of calcium-phosphatized AZ31 magnesium alloy in 0.9 % NaCl solution.

    Science.gov (United States)

    Hadzima, Branislav; Mhaede, Mansour; Pastorek, Filip

    2014-05-01

    Magnesium alloys suffer from their high reactivity in common environments. Protective layers are widely created on the surface of magnesium alloys to improve their corrosion resistance. This article evaluates the influence of a calcium-phosphate layer on the electrochemical characteristics of AZ31 magnesium alloy in 0.9 % NaCl solution. The calcium phosphate (CaP) layer was electrochemically deposited in a solution containing 0.1 M Ca(NO3)2, 0.06 M NH4H2PO4 and 10 ml l(-1) of H2O2. The formed surface layer was composed mainly of brushite [(dicalcium phosphate dihidrate (DCPD)] as proved by energy-dispersive X-ray analysis. The surface morphology was observed by scanning electron microscopy. Immersion test was performed in order to observe degradation of the calcium phosphatized surfaces. The influence of the phosphate layer on the electrochemical characteristics of AZ31, in 0.9 % NaCl solution, was evaluated by potentiodynamic measurements and electrochemical impedance spectroscopy. The obtained results were analysed by the Tafel-extrapolation method and equivalent circuits method. The results showed that the polarization resistance of the DCPD-coated surface is about 25 times higher than that of non-coated surface. The CaP electro-deposition process increased the activation energy of corrosion process.

  12. The use of RANKL-coated brushite cement to stimulate bone remodelling.

    Science.gov (United States)

    Le Nihouannen, Damien; Hacking, S Adam; Gbureck, Uwe; Komarova, Svetlana V; Barralet, Jake E

    2008-08-01

    Calcium phosphate cements were first proposed as synthetic bone substitutes over two decades ago, however, they are characterised by slow chemical or cellular resorption and a slow osteointegration. In contrast, bone autograft has been shown to stimulate osteoclastogenesis and angiogenesis resulting in active bone remodelling and rapid graft incorporation. Therefore, we aimed to develop a biomaterial able to release a key stimulator of the bone remodelling process, cytokine RANKL. Cylinders of brushite cement, hydroxyapatite cement and sodium alginate were loaded with RANKL either by incorporation into the cement or by coating the material with soluble RANKL. To test the biological activity of these formulations, we assessed their effectiveness in inducing osteoclast formation from RAW 264.7 monocytic cell line. Only brushite and hydroxyapatite cements coated with RANKL allowed for retaining sufficient biological activity to induce osteoclast formation. Most efficient was coating 40 mg cylinder of brushite cement with 800 ng RANKL. We have found that RANKL-coated brushite cement exhibits osteoclastogenic activity for at least 1 month at 37 degrees C. Thus, we developed a formulation of brushite cement with RANKL - a synthetic bone graft that is similar to autografts in its ability to actively induce osteoclastogenesis.

  13. Preparation of micro/nano-fibrous brushite coating on titanium via chemical conversion for biomedical applications

    Science.gov (United States)

    Liu, Bing; Guo, Yong-yuan; Xiao, Gui-yong; Lu, Yu-peng

    2017-03-01

    Calcium phosphate coatings have been applied on the surface of Ti implants to realize better osseointegration. The formation of dicalcium phosphate dihydrate (CaHPO4·2H2O), mineralogically named brushite on pure Ti substrate has been investigated via chemical conversion method. Coating composition and microstructure have been investigated by X-ray diffractometer, Fourier transform infrared spectrometer and field emission scanning electron microscope. The results reveal that the coatings are composed of high crystalline brushite with minor scholzite (CaZn2(PO4)2·2H2O). A micro/nano-scaled fibrous morphology can be produced in the acidic chemical conversion bath with pH 5.00. The surface of the fibrous brushite coating exhibits high hydrophilicity and corrosion resistance in the simulated body fluid. The osteoblast cells grow and spread actively on the coated samples and the proliferation numbers and alkaline phosphate activities of the cells improve significantly compared to the uncoated Ti. It is suggested that the micro/nano-fibrous brushite coating can be a potential approach to improve the osteoinductivity and osteoconductivity of Ti implant, due to its similarity in morphology and dimension to inorganic components of biological hard tissues, and favorable responses to the osteoblasts.

  14. Molecular mechanism of crystallization impacting calcium phosphate cements

    Energy Technology Data Exchange (ETDEWEB)

    Giocondi, J L; El-Dasher, B S; Nancollas, G H; Orme, C A

    2009-05-31

    theoretical modeling. The question changes from 'What types of molecules will inhibit brushite growth' to 'What type of molecule will interact with the [10-1]{sub Cc} step?' Similarly, to increase resorption rate, it would be most efficacious to target the slow moving [-100] step, perhaps by targeting the hydroxyl group which seem to stabilize this step compared to its otherwise similar mirror, [100]. In short, there are a number of opportunities where molecular scale imaging can provide new information that has the prospect to aid in optimizing calcium phosphate cements.

  15. Effect of silica gel on the cohesion, properties and biological performance of brushite cement.

    Science.gov (United States)

    Alkhraisat, Mohammad Hamdan; Rueda, Carmen; Jerez, Luis Blanco; Tamimi Mariño, Faleh; Torres, Jesus; Gbureck, Uwe; Lopez Cabarcos, Enrique

    2010-01-01

    The cohesion of calcium phosphate cements can be improved by the addition of substances to either the solid or liquid phase during the setting reaction. This study reports the effect of silica gel on brushite cement cohesion. The cement was prepared using a mixture of beta-tricalcium phosphate (beta-TCP) and monocalcium phosphate monohydrate as the solid phase, while the liquid phase comprised carboxylic acids silica gel. This cement presents a shorter final setting time (FST), better cohesion and higher amount of unreacted beta-TCP than the cement prepared without silica gel. Furthermore, in vivo experiments using rabbits as an animal model showed that after 8 weeks of implantation cements modified with silica gel showed a similar new bone formation volume and more remaining graft in comparison with unmodified cements. Thus, the silica gel could be efficiently applied to reduce cement disintegration and to decrease the resorption rate of brushite cements.

  16. Preparation and characterization of bioceramics produced from calcium phosphate cements

    Energy Technology Data Exchange (ETDEWEB)

    Andriotis, O.; Katsamenis, O.L. [Department of Materials Science, University of Patras, 26504, Patras (Greece); Mouzakis, D.E. [Technological Educational Institute of Larisa, Department of Mechanical Engineering, T.E.I of Larissa, 411 10, Larissa (Greece); Bouropoulos, N. [Foundation for Research and Technology, Hellas, Institute of Chemical Engineering and High Temperature Chemical Processes, FORTH/ICE-HT, P.O. Box 1414, 26504 Rio Patras (Greece)

    2010-03-15

    The present work reports a method for preparing calcium phosphate ceramics by calcination of calcium phosphate cements composed mainly of calcium deficient hydroxyapatite (CDHA). It was found that hardened cements calcinied at temperatures from to 600 to 1300 C were transformed to tricalcium phosphates. Moreover the compressive strength was determined and porosity was estimated as a function of the calcination temperature. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  17. Topotactic exchange and intercalation of calcium phosphate

    Science.gov (United States)

    Lima, Cicero B. A.; Airoldi, Claudio

    2004-11-01

    The precursor (NH 4) 2Ca(H 2PO 4) 2ṡH 2O (CaAP) compound was obtained by combining a calcium chloride solution with dibasic ammonium phosphate. After submitting it to a thermal treatment, crystalline calcium phosphate, Ca(H 2PO 4) 2ṡH 2O (CaP) was isolated. X-ray diffraction patterns for this compound indicated good crystallinity, with a peak at 2θ=12.8°, to give an interlamellar distance of 697 pm, which changed to 1550 pm, when the reaction employed phenylphosphonic acid, and to 1514 pm when intercalated with methylamine. Phosphorus and calcium analysis from colorimetric and gravimetric methods gave for CaP 24.2 and 15.8%, respectively, to yield a P:Ca molar ratio equal to two. The phosphorus nuclear magnetic resonance presented a peak centered at -1.23 ppm, in agreement with the existence of phosphate groups in protonated form. CaAP showed a mass loss of 21.2% in the 466 to 541 K interval due to ammonia and water elimination to yield Ca(PO 3) 3, and CaP can be dehydrated at 440 K for 6 h. A topotactical exchange occurred when CaP is intercalated with methylamine or reacted with phenylphosphonic acid to yield the phosphonate compound and the infrared spectrum of the resulting compound clearly showed the presence of PO 4 and PO 3 groups. The topotactic exchange was also demonstrated by X-ray diffractometry in following the stages of decomposition from 527 to 973 K.

  18. Preparation and Characterization of Injectable Brushite Filled-Poly (Methyl Methacrylate Bone Cement

    Directory of Open Access Journals (Sweden)

    Lucas C. Rodriguez

    2014-09-01

    Full Text Available Powder-liquid poly (methyl methacrylate (PMMA bone cements are widely utilized for augmentation of bone fractures and fixation of orthopedic implants. These cements typically have an abundance of beneficial qualities, however their lack of bioactivity allows for continued development. To enhance osseointegration and bioactivity, calcium phosphate cements prepared with hydroxyapatite, brushite or tricalcium phosphates have been introduced with rather unsuccessful results due to increased cement viscosity, poor handling and reduced mechanical performance. This has limited the use of such cements in applications requiring delivery through small cannulas and in load bearing. The goal of this study is to design an alternative cement system that can better accommodate calcium-phosphate additives while preserving cement rheological properties and performance. In the present work, a number of brushite-filled two-solution bone cements were prepared and characterized by studying their complex viscosity-versus-test frequency, extrusion stress, clumping tendency during injection through a syringe, extent of fill of a machined void in cortical bone analog specimens, and compressive strength. The addition of brushite into the two-solution cement formulations investigated did not affect the pseudoplastic behavior and handling properties of the materials as demonstrated by rheological experiments. Extrusion stress was observed to vary with brushite concentration with values lower or in the range of control PMMA-based cements. The materials were observed to completely fill pre-formed voids in bone analog specimens. Cement compressive strength was observed to decrease with increasing concentration of fillers; however, the materials exhibited high enough strength for consideration in load bearing applications. The results indicated that partially substituting the PMMA phase of the two-solution cement with brushite at a 40% by mass concentration provided the best

  19. Water-Soluble Cellulose Derivatives Are Sustainable Additives for Biomimetic Calcium Phosphate Mineralization

    Directory of Open Access Journals (Sweden)

    Andreas Taubert

    2016-10-01

    Full Text Available The effect of cellulose-based polyelectrolytes on biomimetic calcium phosphate mineralization is described. Three cellulose derivatives, a polyanion, a polycation, and a polyzwitterion were used as additives. Scanning electron microscopy, X-ray diffraction, IR and Raman spectroscopy show that, depending on the composition of the starting solution, hydroxyapatite or brushite precipitates form. Infrared and Raman spectroscopy also show that significant amounts of nitrate ions are incorporated in the precipitates. Energy dispersive X-ray spectroscopy shows that the Ca/P ratio varies throughout the samples and resembles that of other bioinspired calcium phosphate hybrid materials. Elemental analysis shows that the carbon (i.e., polymer contents reach 10% in some samples, clearly illustrating the formation of a true hybrid material. Overall, the data indicate that a higher polymer concentration in the reaction mixture favors the formation of polymer-enriched materials, while lower polymer concentrations or high precursor concentrations favor the formation of products that are closely related to the control samples precipitated in the absence of polymer. The results thus highlight the potential of (water-soluble cellulose derivatives for the synthesis and design of bioinspired and bio-based hybrid materials.

  20. Preparation, Physical-Chemical Characterization, and Cytocompatibility of Polymeric Calcium Phosphate Cements

    Science.gov (United States)

    Khashaba, Rania M.; Moussa, Mervet; Koch, Christopher; Jurgensen, Arthur R.; Missimer, David M.; Rutherford, Ronny L.; Chutkan, Norman B.; Borke, James L.

    2011-01-01

    Aim. Physicochemical mechanical and in vitro biological properties of novel formulations of polymeric calcium phosphate cements (CPCs) were investigated. Methods. Monocalcium phosphate, calcium oxide, and synthetic hydroxyapatite were combined with either modified polyacrylic acid, light activated polyalkenoic acid, or polymethyl vinyl ether maleic acid to obtain Types I, II, and III CPCs. Setting time, compressive and diametral strength of CPCs was compared with zinc polycarboxylate cement (control). Specimens were characterized using X-ray diffraction, scanning electron microscopy, and infrared spectroscopy. In vitro cytotoxicity of CPCs and control was assessed. Results. X-ray diffraction analysis showed hydroxyapatite, monetite, and brushite. Acid-base reaction was confirmed by the appearance of stretching peaks in IR spectra of set cements. SEM revealed rod-like crystals and platy crystals. Setting time of cements was 5–12 min. Type III showed significantly higher strength values compared to control. Type III yielded high biocompatibility. Conclusions. Type III CPCs show promise for dental applications. PMID:21941551

  1. Preparation, Physical-Chemical Characterization, and Cytocompatibility of Polymeric Calcium Phosphate Cements

    Directory of Open Access Journals (Sweden)

    Rania M. Khashaba

    2011-01-01

    Full Text Available Aim. Physicochemical mechanical and in vitro biological properties of novel formulations of polymeric calcium phosphate cements (CPCs were investigated. Methods. Monocalcium phosphate, calcium oxide, and synthetic hydroxyapatite were combined with either modified polyacrylic acid, light activated polyalkenoic acid, or polymethyl vinyl ether maleic acid to obtain Types I, II, and III CPCs. Setting time, compressive and diametral strength of CPCs was compared with zinc polycarboxylate cement (control. Specimens were characterized using X-ray diffraction, scanning electron microscopy, and infrared spectroscopy. In vitro cytotoxicity of CPCs and control was assessed. Results. X-ray diffraction analysis showed hydroxyapatite, monetite, and brushite. Acid-base reaction was confirmed by the appearance of stretching peaks in IR spectra of set cements. SEM revealed rod-like crystals and platy crystals. Setting time of cements was 5–12 min. Type III showed significantly higher strength values compared to control. Type III yielded high biocompatibility. Conclusions. Type III CPCs show promise for dental applications.

  2. Preparation of Porous Calcium Phosphate Bioceramic

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Porous calcium phosphate ceramics were prepared by slip casting and molding method respectively. By these two different methods, different microstructures can be got. By slip casting method, the pore size was 100- 350μm and 20- 80μm; pores were opened, interconnected and ball-like; the grain size was 2- 4 μm.By molding method, the pore size was 100-500 μm and 1-10μm; the grain size was 2-8μm. By slip casting method regular and interconnected pores can be got. By molding method the porosity and strength can be adjusted easily.

  3. Characterization of a new composite PMMA-HA/Brushite bone cement for spinal augmentation.

    Science.gov (United States)

    Aghyarian, Shant; Rodriguez, Lucas C; Chari, Jonathan; Bentley, Elizabeth; Kosmopoulos, Victor; Lieberman, Isador H; Rodrigues, Danieli C

    2014-11-01

    Calcium phosphate fillers have been shown to increase cement osteoconductivity, but have caused drawbacks in cement properties. Hydroxyapatite and Brushite were introduced in an acrylic two-solution cement at varying concentrations. Novel composite bone cements were developed and characterized using rheology, injectability, and mechanical tests. It was hypothesized that the ample swelling time allowed by the premixed two-solution cement would enable thorough dispersion of the additives in the solutions, resulting in no detrimental effects after polymerization. The addition of Hydroxyapatite and Brushite both caused an increase in cement viscosity; however, these cements exhibited high shear-thinning, which facilitated injection. In gel point studies, the composite cements showed no detectable change in gel point time compared to an all-acrylic control cement. Hydroxyapatite and Brushite composite cements were observed to have high mechanical strengths even at high loads of calcium phosphate fillers. These cements showed an average compressive strength of 85 MPa and flexural strength of 65 MPa. A calcium phosphate-containing cement exhibiting a combination of high viscosity, pseudoplasticity and high mechanical strength can provide the essential bioactivity factor for osseointegration without sacrificing load-bearing capability.

  4. Hybrid calcium phosphate coatings for implants

    Science.gov (United States)

    Malchikhina, Alena I.; Shesterikov, Evgeny V.; Bolbasov, Evgeny N.; Ignatov, Viktor P.; Tverdokhlebov, Sergei I.

    2016-08-01

    Monophasic biomaterials cannot provide all the necessary functions of bones or other calcined tissues. It is necessary to create for cancer patients the multiphase materials with the structure and composition simulating the natural bone. Such materials are classified as hybrid, obtained by a combination of chemically different components. The paper presents the physical, chemical and biological studies of coatings produced by hybrid technologies (HT), which combine primer layer and calcium phosphate (CaP) coating. The first HT type combines the method of vacuum arc titanium primer layer deposition on a stainless steel substrate with the following micro-arc oxidation (MAO) in phosphoric acid solution with addition of calcium compounds to achieve high supersaturated state. MAO CaP coatings feature high porosity (2-8%, pore size 5-7 µm) and surface morphology with the thickness greater than 5 µm. The thickness of Ti primer layer is 5-40 µm. Amorphous MAO CaP coating micro-hardness was measured at maximum normal load Fmax = 300 mN. It was 3.1 ± 0.8 GPa, surface layer elasticity modulus E = 110 ± 20 GPa, roughness Ra = 0.9 ± 0.1 µm, Rz = 7.5 ± 0.2 µm, which is less than the titanium primer layer roughness. Hybrid MAO CaP coating is biocompatible, able to form calcium phosphates from supersaturated body fluid (SBF) solution and also stimulates osteoinduction processes. The second HT type includes the oxide layer formation by thermal oxidation and then CaP target radio frequency magnetron sputtering (RFMS). Oxide-RFMS CaP coating is a thin dense coating with good adhesion to the substrate material, which can be used for metal implants. The RFMS CaP coating has thickness 1.6 ± 0.1 µm and consists of main target elements calcium and phosphorus and Ca/P ratio 2.4. The second HT type can form calcium phosphates from SBF solution. In vivo study shows that hybrid RFMS CaP coating is biocompatible and produces fibrointegration processes.

  5. Seed selections for crystallization of calcium phosphate for phosphorus recovery

    Institute of Scientific and Technical Information of China (English)

    SONG Yong-hui; Dietfried DONNERT; Ute BERG; Peter G. WEIDLER; Rolf NUEESCH

    2007-01-01

    Seed induces and promotes the crystallization of calcium phosphate, and acts as carrier of the recovered phosphorus (P). In order to select suitable seed for P recovery from wastewater, three seeds including Apatite (AP), Juraperle (JP) and phosphate-modified Juraperle (M-JP) were tested and compared. Batch and fixed-bed column experiments of seeded crystallization of calcium phosphate were undertaken by using synthetic wastewater with 10 mg/L P phosphate. It shows that AP has bad enduring property in the crystallization process, while JP has better performance for multiple uses, and M-JP is a hopeful seed for P recovery by crystallization of calcium phosphate.

  6. Fabrications of zinc-releasing biocement combining zinc calcium phosphate to calcium phosphate cement.

    Science.gov (United States)

    Horiuchi, Shinya; Hiasa, Masahiro; Yasue, Akihiro; Sekine, Kazumitsu; Hamada, Kenichi; Asaoka, Kenzo; Tanaka, Eiji

    2014-01-01

    Recently, zinc-releasing bioceramics have been the focus of much attention owing to their bone-forming ability. Thus, some types of zinc-containing calcium phosphate (e.g., zinc-doped tricalcium phosphate and zinc-substituted hydroxyapatite) are examined and their osteoblastic cell responses determined. In this investigation, we studied the effects of zinc calcium phosphate (ZCP) derived from zinc phosphate incorporated into calcium phosphate cement (CPC) in terms of its setting reaction and MC3T3-E1 osteoblast-like cell responses. Compositional analysis by powder X-ray diffraction analysis revealed that HAP crystals were precipitated in the CPC containing 10 or 30wt% ZCP after successfully hardening. However, the crystal growth observed by scanning electron microscopy was delayed in the presence of additional ZCP. These findings indicate that the additional zinc inhibits crystal growth and the conversion of CPC to the HAP crystals. The proliferation of the cells and alkaline phosphatase (ALP) activity were enhanced when 10wt% ZCP was added to CPC. Taken together, ZCP added CPC at an appropriate fraction has a potent promotional effect on bone substitute biomaterials.

  7. Effect of albumin on brushite transformation to hydroxyapatite.

    Science.gov (United States)

    Xie, J; Riley, C; Chittur, K

    2001-12-05

    Brushite (CaHPO(4) x 2H(2)O) is a precursor to hydroxyapatite [HA, Ca(5)(PO(4))(3)OH]. It has been shown that a modified form of brushite, with potassium substituting for calcium at specific sites, demonstrated accelerated transformation to HA when exposed to nonproteinaceous Hanks' balanced aqueous salt solutions (HBSS). The biocompatibility of a transforming material is related to cellular response to the process, which is initiated by protein adsorption. The effect of adsorbed protein on the kinetics and chemistry of brushite transformation to HA, when exposed to HBSS containing bovine serum albumin (BSA), was examined using Fourier transform IR spectroscopy, X-ray diffraction, and energy dispersive spectrometry techniques. The effect of solution pH was also studied. Results show that, in the presence of a protein-free environment, transformation is faster in buffered medium than in nonbuffered medium. Moreover, curve fitting and second derivatives of the IR spectra show that some bands shift depending on whether the brushite transforms in a buffered or nonbuffered medium. Therefore, variation in pH affects both transformation rate and the associated chemistry. The presence of BSA in either buffered or nonbuffered medium retards the transformation in comparison to the corresponding BSA-free medium. The extent of this retardation increases with the increase in bulk concentration of BSA but does not alter the transformation chemistry. This suggests the retardation on the transformation rate is due to BSA adsorption coverage on the calcium phosphate ceramic. This may be due to the shielding of Ca(2+) and PO(4)(-3) sites, preventing their interaction with the HBSS.

  8. Surface induced constant composition crystal growth kinetics studies. The brushite gypsum system

    Science.gov (United States)

    Hina, A.; Nancollas, G. H.; Grynpas, M.

    2001-02-01

    The possible oriented growth of one crystalline phase on the surface of another is especially important in systems containing both phosphate and sulfate salts of calcium. Whether the overgrowth results from a true epitaxial relationship is dependent on factors such as the thermodynamic driving forces and the free energies of the surfaces. Despite the fact that calcium sulfate dihydrate (CSD, gypsum) and calcium hydrogen phosphate dihydrate (DCPD, brushite) show many crystallographic and structural analogies, their surface reactions are quite different. The nucleation and growth of gypsum on brushite surfaces has been investigated in supersaturated solutions of calcium sulfate dihydrate at 25.0°C using the constant composition (CC) method. During the kinetics experiments, the harvested solid phases were examined by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive X-ray analysis (EDS). Induction periods, τ, preceding the initial formation of gypsum crystals at the brushite surfaces, varied markedly with relative supersaturation, σ. A thin layer wicking method was used to investigate the interfacial free energies of the growing phases, and these data were also calculated from the kinetics results. The interfacial free energy, γ, estimated from initial growth rates was 8.4 mJ m -2, while that calculated from the induction times was 8.9 mJ m -2. These values were in agreement with those determined directly using thin layer wicking.

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

    Science.gov (United States)

    Roberts, J E; Heughebaert, M; Heughebaert, J C; Bonar, L C; Glimcher, M J; Griffin, R G

    1991-12-01

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

  10. Dual-setting brushite-silica gel cements.

    Science.gov (United States)

    Geffers, Martha; Barralet, Jake E; Groll, Jürgen; Gbureck, Uwe

    2015-01-01

    The current study describes a dual-mechanism-setting cement that combines a brushite-forming cement paste with a second inorganic silica-based precursor. Materials were obtained by pre-hydrolyzing tetraethyl orthosilicate (TEOS) under acidic conditions following the addition of a calcium phosphate cement (CPC) powder mixed of β-tricalcium phosphate and monocalcium phosphate. Cement setting occurred by a dissolution-precipitation process, while changes in pH during setting simultaneously initiated the condensation reaction of the hydrolyzed TEOS. This resulted in an interpenetrating phase composite material in which the macropores of the CPC were infiltrated by the microporous silica gel, leading to a higher density and a compressive strength ∼5-10 times higher than the CPC reference. This also altered the release of vancomycin as a model drug, whereby in contrast to the quantitative release from the CPC reference, 25% of the immobilized drug remained in the composite matrix. By varying the TEOS content in the composite, the cement phase composition could be controlled to form either brushite, anhydrous monetite or a biphasic mixture of both. The composites with the highest silicate content showed a cell proliferation similar to a hydroxyapatite reference with a significantly higher activity per cell. Surprisingly, the biological response did not seem to be attributed to the released silicate ions, but to the release of phosphate and the adsorption of magnesium ions from the cell culture medium.

  11. Minimally invasive maxillofacial vertical bone augmentation using brushite based cements.

    Science.gov (United States)

    Tamimi, Faleh; Torres, Jesus; Lopez-Cabarcos, Enrique; Bassett, David C; Habibovic, Pamela; Luceron, Elena; Barralet, Jake E

    2009-01-01

    An ideal material for maxillofacial vertical bone augmentation procedures should not only be osteoconductive, biocompatible and mechanically strong, but should also be applied using minimally invasive procedures and remain stable with respect to the original bone surfaces. This way, implant exposure and infection might be reduced and good mechanical stability may be achieved. Calcium phosphate cements are proven biocompatible and osteoconductive materials that can be injected using minimally invasive procedures. Among these cements, brushite based cements have the added advantage of being biodegradable in vivo. Therefore, this material has the potential for use in the aforementioned procedures. An in vivo study was performed in rabbits to evaluate the potential use of brushite cements in minimally invasive maxillofacial vertical bone augmentation procedures. In this study, we injected self-setting brushite cements on the subperiosteal bone surface using a minimally invasive tunnelling technique. The cement pastes were stable on the bone surface and hardened soon after they were injected thereby negating the need for additional supports such as membranes or meshes. The animals were sacrificed 8 weeks after the intervention and histological observations revealed signs of successful vertical bone augmentation. Therefore, we have demonstrated a minimally invasive vertical bone augmentation procedure that is an attractive alternative to current surgical procedures in terms of increased simplicity, reduced trauma, and lower cost of surgery.

  12. Odontoblast phosphate and calcium transport in dentinogenesis.

    Science.gov (United States)

    Lundquist, Patrik

    2002-01-01

    It has been suggested that odontoblasts are instrumental in translocating Ca2+ and inorganic phosphate (Pi) ions during the mineralization of dentin. The aim of this thesis was, therefore, to study the expression of components of the transcellular ion transport system, Na+/Ca2+ exchangers and Na(+)-Pi contransporters, in odontoblastic and osteoblastic cells. Their activity was assayed in osteoblast-like cells and in the recently developed MRPC-1 odontoblast-like cell line. To assess the relationship between ion transport and mineralization, Ca2+ and Pi uptake activities were determined in mineralizing cultures of MRPC-1 cells. Osteoblastic and odontoblastic cells showed an identical expression pattern of Na+/Ca2+ exchanger splice-variants, NCX1.3, NCX1.7 and NCX1.10, derived from the NCX1 gene, while NCX2 was not expressed. The cells showed a high sodium-dependent calcium extrusion activity. Regarding Na(+)-Pi cotransporter expression, Glvr-1, Ram-1 and the two high capacity cotransporters Npt-2a and Npt-2b were found to be expressed in odontoblasts and MRPC-1 cells. Osteoblast-like cells differed from this in expressing the Npt-1 but not the Ram-1 gene but were otherwise identical to the odontoblastic cells. Odontoblast-like cells exhibited almost twice the sodium-dependent Pi uptake activity of osteoblast-like cells. The presence of NaPi-2a and NaPi-2b, gene products of Npt-2a and Npt-2b, was verified in vivo by immunohistochemistry on mouse teeth. Both cotransporters could be detected in fully differentiated, polarized odontoblasts but not in preodontoblasts prior to dentin formation. Both cotransporters were detected in adjacent bone and in ameloblasts. Studying ion uptake in mineralizing MRPC-1 cultures, large changes were detected concomitant with the onset of mineral formation, when phosphate uptake increased by 400% while calcium uptake started to decline. The increase in Pi uptake was found to be due to activation of the NaPi-2a cotransporter. MRPC-1 cells

  13. Pathogenic Mineralization of Calcium Phosphate on Human Heart Valves

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    When calcium phosphate forms in soft tissues such as blood vessels and heart valves, it causes disease. The abnormal formation of calcium phosphate is called pathogenic mineralization or pathogenic calcification. Cases of rheumatic heart disease (RHD) always occur with fibrotic and calcified tissue of heart valve. In this article, samples taken from calcified human heart valves were studied. The characterization was performed by scanning electronic micrascope, X-ray Diffraction and transmission electron microscopy with selective diffraction patterns. It is found for the first time that calcium phosphate grains existing in the calcified human heart valves contain octacalcium phosphate (OCP).

  14. Calcium phosphate/porous silicon biocomposites prepared by cyclic deposition methods: Spin coating vs electrochemical activation

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez-Montelongo, J., E-mail: jacobo.hernandez@uam.es [Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Gallach, D.; Naveas, N.; Torres-Costa, V. [Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Climent-Font, A. [Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Centro de Microanálisis de Materiales (CMAM), Universidad Autónoma de Madrid, Madrid 28049 (Spain); García-Ruiz, J.P. [Departamento de Biología Molecular, Universidad Autónoma de Madrid, Cantoblanco, Madrid 28049 (Spain); Manso-Silvan, M. [Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain)

    2014-01-01

    Porous silicon (PSi) provides an excellent platform for bioengineering applications due to its biocompatibility, biodegradability, and bioresorbability. However, to promote its application as bone engineering scaffold, deposition of calcium phosphate (CaP) ceramics in its hydroxyapatite (HAP) phase is in progress. In that sense, this work focuses on the synthesis of CaP/PSi composites by means of two different techniques for CaP deposition on PSi: Cyclic Spin Coating (CSC) and Cyclic Electrochemical Activation (CEA). Both techniques CSC and CEA consisted on alternate Ca and P deposition steps on PSi. Each technique produced specific morphologies and CaP phases using the same independent Ca and P stem-solutions at neutral pH and at room temperature. The brushite (BRU) phase was favored with the CSC technique and the hydroxyapatite (HAP) phase was better synthesized using the CEA technique. Analyses by elastic backscattering spectroscopy (EBS) on CaP/PSi structures synthesized by CEA supported that, by controlling the CEA parameters, an HAP coating with the required Ca/P atomic ratio of 1.67 can be promoted. Biocompatibility was evaluated by bone-derived progenitor cells, which grew onto CaP/PSi prepared by CSC technique with a long-shaped actin cytoskeleton. The density of adhered cells was higher on CaP/PSi prepared by CEA, where cells presented a normal morphological appearance and active mitosis. These results can be used for the design and optimization of CaP/PSi composites with enhanced biocompatibility for bone-tissue engineering. - Highlights: • Proposed cyclic methods produce specific morphologies and CaP phases in biocomposites. • The brushite phase is favored in the biocomposite produced by Cyclic Spin Coating. • The hydroxyapatite phase is favored in the biocomposite produced by Cyclic Electrochemical Activation. • The Ca/P atomic ratio of hydroxyapatite was validated by elastic backscattering spectroscopy. • Cells grown showed morphological and

  15. Preparation and Characterization of Porous Calcium Phosphate Bioceramics

    Institute of Scientific and Technical Information of China (English)

    Honglian Dai; Xinyu Wang; Yinchao Han; Xin Jiang; Shipu Li

    2011-01-01

    β-tricalcium phosphate (β-TCP) powder and Na2O-CaO-MgO-P2O5 glass binder were synthesized and mixed, and then the biodegradable porous calcium phosphate ceramics were successfully prepared by foaming and sintering at 850℃. The as-prepared ceramics possess a high porosity with partial three-dimension interconnected macro- and micro-pores. As in vitro experiment testified, the calcium phosphate ceramics (CPCs) has good degradability.

  16. Heterogeneous nucleation of calcium phosphate salts at a solid/liquid interface examined by scanning angle reflectometry

    Science.gov (United States)

    Ngankam, P. A.; Schaaf, P.; Voegel, J. C.; Cuisinier, F. J. G.

    1999-03-01

    Mineralization of calcium phosphate salts at a solid/liquid silica interface was examined by means of scanning angle reflectometry (SAR). A critical supersaturation of 7.60±0.15 mM was found to be the lowest calcium phosphate concentration at pH 6.85 at which the reflectivity at the Brewster angle started to vary. The analyses of the signals by mean of the homogeneous isotropic layer model led to layer thicknesses of about 3.5 μm also characterized by very low mean refractive index increments. These observations were completed by complementary experiments. Scanning and transmission electron microscopy led to similar layer thicknesses with crystallites dispersed in the whole layer confirming thus SAR results. X-ray analyses showed a presence of brushite (DCPD) at the silica interface. A pH of 5.44 was estimated for the acidic silica interface for which DCPD is nucleated after addition of 7.60±0.15 mM calcium and phosphate. However, at this pH value, the solution is largely supersaturated with respect to hydroxyapatite (HAP theoretical saturating concentration: 1.37 mM). A faster growth of DCPD crystals compared to HAP crystals is thus assumed to explain our observations.

  17. Effect of the calcium to phosphate ratio of tetracalcium phosphate on the properties of calcium phosphate bone cement.

    Science.gov (United States)

    Burguera, Elena F; Guitian, Francisco; Chow, Laurence C

    2008-06-01

    Six different tetracalcium phosphate (TTCP) products were synthesized by solid state reaction at high temperature by varying the overall calcium to phosphate ratio of the synthesis mixture. The objective was to evaluate the effect of the calcium to phosphate ratio on a TTCP-dicalcium phosphate dihydrate (DCPD) cement. The resulting six TTCP-DCPD cement mixtures were characterized using X-ray diffraction analysis, scanning electron microscopy, and pH measurements. Setting times and compressive strength (CS) were also measured. Using the TTCP product with a Ca/P ratio of 2.0 resulted in low strength values (25.61 MPa) when distilled water was used as the setting liquid, even though conversion to hydroxyapatite was not prevented, as confirmed by X-ray diffraction. The suspected CaO presence in this TTCP may have affected the cohesiveness of the cement mixture but not the cement setting reaction, however no direct evidence of CaO presence was found. Lower Ca/P ratio products yielded cements with CS values ranging from 46.7 MPa for Ca/P ratio of 1.90 to 38.32 MPa for Ca/P ratio of 1.85. When a dilute sodium phosphate solution was used as the setting liquid, CS values were 15.3% lower than those obtained with water as the setting liquid. Setting times ranged from 18 to 22 min when water was the cement liquid and from 7 to 8 min when sodium phosphate solution was used, and the calcium to phosphate ratio did not have a marked effect on this property.

  18. Characterization of calcium phosphate deposited on valve metal by anodic oxidation with polarity inversion.

    Science.gov (United States)

    Okawa, Seigo; Homma, Kikuo; Kanatani, Mitsugu; Watanabe, Kouichi

    2009-07-01

    Electrochemical deposition of calcium phosphate (CAP) on valve metals such as Ta, Nb, and Zr, was performed by anodic oxidation with alternate polarity inversion at an applied 20 VDC. A saturated hydroxyapatite(HAP)-phosphoric acid solution (pH 3) was used as the electrolyte. FTIR, XRD, and XPS were employed to investigate the detailed characteristics of the deposition. HAP was precipitated on Ta; HAP including brushite and monetite on Nb; and HAP and monetite on Zr. The Ca/P atomic ratios were 1.3-1.5 by XPS, and HPO(4)(2- )bands were detected on Ta by FTIR. Therefore, the HAP precipitated on Ta was a Ca-deficient HAP. In addition, the XPS spectra of the specimens showed that phosphate ions were incorporated into the anodic oxide film. Deposits with nano-grain size were observed by AFM. The results confirmed that CAP with nano-grain size was deposited on valve metals by the anodic oxidation with polarity inversion.

  19. Mechanical and In Vitro Biocompatibility of Brushite Cement Modified by Polyethylene Glycol

    OpenAIRE

    2012-01-01

    Brushite (dicalcium phosphate dihydrate, DCPD) cement, owing to its high solubility in physiological condition and ability to guide new bone formation, is widely used to treat bone defects. In the present study, we have evaluated the effects of poly ethylene glycol (PEG) addition on the setting time, compressive strength and in vitro biocompatibility of brushite cement. The brushite cements were prepared by mixing β-tricalcium phosphate [β-TCP, Ca3(PO4)2] and monocalcium phosphate monohydrate...

  20. Injectable bioactive calcium-magnesium phosphate cement for bone regeneration.

    Science.gov (United States)

    Wu, Fan; Su, Jiacan; Wei, Jie; Guo, Han; Liu, Changsheng

    2008-12-01

    Novel injectable and degradable calcium-magnesium phosphate cement (CMPC) with rapid-setting characteristic was developed by the introduction of magnesium phosphate cement (MPC) into calcium phosphate cement (CPC). The calcium-magnesium phosphate cement prepared under the optimum P/L ratio exhibited good injectability and desired workability. It could set within 10 min at 37 degrees C in 100% relative humidity and the compressive strength could reach 47 MPa after setting for 48 h, indicating that the prepared cement has relatively high initial mechanical strength. The results of in vitro degradation experiments demonstrated the good degradability of the injectable CMPC, and its degradation rate occurred significantly faster than that of pure CPC in simulated body fluid (SBF) solution. It can be concluded that the novel injectable calcium-magnesium phosphate cement is highly promising for a wide variety of clinical applications, especially for the development of minimally invasive techniques.

  1. Factors influencing calcium phosphate cement shelf-life.

    Science.gov (United States)

    Gbureck, Uwe; Dembski, Sofia; Thull, Roger; Barralet, Jake E

    2005-06-01

    Long-term stability during storage (shelf-life) is one major criterion for the use of a material as medical device. This study aimed to investigate the ageing process of beta-tricalcium phosphate/monocalcium phosphate cement powders when stored in sealed containers at ambient conditions. This kind of cement type is of interest because it is forming dicalcium phosphate dihydrate (brushite) when set, which is in contrast to hydroxyapatite resorbable in physiological conditions. The stability of cements was checked by either measuring the phase composition of powders as well as the setting time and compressive strength when mixed with sodium citrate as liquid. Critical factors influencing ageing were found to be temperature, humidity and the mixing regime of the powders. Mechanically mixed cement powders which were stored in normal laboratory atmosphere (22 degrees C, 60% rel. humidity) converted to dicalcium phosphate anhydrous (monetite) within a few days; this could be mechanistically related to a dissolution/precipitation process since humidity condensed on the particles' surfaces and acted as reaction medium. Various storage conditions were found to be effective in prolonging cement stability which were in order of effectiveness: adding solid citric acid retardant>dry argon atmosphere=gentle mixing (minimal mechanical energy input) low temperature.

  2. Effect of curing conditions on the dimensional and thermal stability of calcium phosphate cement for elevated temperature applications

    Energy Technology Data Exchange (ETDEWEB)

    Blom, Johan [Vrije Universiteit Brussel, Department of Mechanics of Materials and Constructions, Pleinlaan 2, Brussels 1050 (Belgium); Rahier, Hubert [Vrije Universiteit Brussel, Research Group of Physical Chemistry and Polymer Sciences, Pleinlaan 2, Brussels 1050 (Belgium); Wastiels, Jan, E-mail: Jan.Wastiels@vub.ac.be [Vrije Universiteit Brussel, Department of Mechanics of Materials and Constructions, Pleinlaan 2, Brussels 1050 (Belgium)

    2014-12-15

    Calcium phosphate cements (CPCs) are attractive materials for elevated temperature applications, like moulds to process thermoplastics up to 300 °C. The CPC resulting from the reaction of wollastonite with phosphoric acid cured at room temperature however contains hydrated phases like brushite, and is thus not stable when exposed to temperatures above 200 °C. A non-contact method based on digital image correlation demonstrated that isothermal curing at 60 °C reduces the thermal shrinkage up to 300 °C by 25%. This curing method results in the direct formation of the more stable monetite in a shorter curing time. The correlated results of TGA, pH of the filtration water, and DSC analysis on partially cured material indicate this. XRD diffractograms and SEM images in combination with EDX show the evolution of the transformation of wollastonite into monetite, and the structure and morphology of the formed material.

  3. Long-Term In Vitro Degradation of a High-Strength Brushite Cement in Water, PBS, and Serum Solution

    OpenAIRE

    2015-01-01

    Bone loss and fractures may call for the use of bone substituting materials, such as calcium phosphate cements (CPCs). CPCs can be degradable, and, to determine their limitations in terms of applications, their mechanical as well as chemical properties need to be evaluated over longer periods of time, under physiological conditions. However, there is lack of data on how the in vitro degradation affects high-strength brushite CPCs over longer periods of time, that is, longer than it takes for ...

  4. Long-term in vitro degradation of a high-strength brushite cement in water, PBS, and serum solution

    OpenAIRE

    2015-01-01

    Bone loss and fractures may call for the use of bone substituting materials, such as calcium phosphate cements (CPCs). CPCs can be degradable, and, to determine their limitations in terms of applications, their mechanical as well as chemical properties need to be evaluated over longer periods of time, under physiological conditions. However, there is lack of data on how the in vitro degradation affects high-strength brushite CPCs over longer periods of time, that is, longer than it takes for ...

  5. Raman microspectrometry studies of brushite cement: in vivo evolution in a sheep model.

    Science.gov (United States)

    Penel, G; Leroy, N; Van Landuyt, P; Flautre, B; Hardouin, P; Lemaître, J; Leroy, G

    1999-08-01

    Calcium phosphate hydraulic cements are promising synthetic bone grafting materials. Brushite-based cements were implanted for 6 and 12 months in the distal condyle of sheep femur, and their in vivo evolution was investigated by Raman microspectrometry. This new technique can probe small volumes in the cubic micrometer range. Its resolution allows a very fine analysis of crystalline changes in calcium phosphate mixtures at the microscopic level. First, Raman spectra of pure brushite, monetite, and beta-tricalcium phosphate (beta-TCP) were recorded, in order to set a data base for the basic components of brushite cements. These spectra show significant differences in the vibration mode v1 for the phosphate ion (988 and 878 cm(-1) for brushite, 988 and 900 cm(-1) for monetite, 968 and 948 cm(-1) for beta-TCP). These differences are strong enough as to allow the qualitative and quantitative analysis of these crystalline phases in the cement. Implanted sheep femur samples were harvested after 24 and 52 weeks post-op, and prepared for Raman analysis in the form of 1-mm-thick sections. Implants at 24 weeks show a core of residual cement isolated from the surrounding bone by fibroconnective tissue. No trace of brushite was detected by micro-Raman analysis in this area, but instead, a mixture of beta-TCP and Type-B carbonated apatite, the latter being very close in composition and structure to the mineral fraction of normal bone in the vicinity of the implant. Implants recovered after 52 weeks show a decrease of the bone/residual cement perimeter, whereas new trabeculations are formed in the implanted zone; the small amounts of residual cement still present are substantially transformed into Type-B carbonated apatite containing small amounts of proteins. In the same area, some beta-TCP particles are also detected showing that, contrary to brushite, the excess beta-TCP originally present in the cement is not completely metabolized. In the implanted zone already converted

  6. Accelerated transformation of brushite to octacalcium phosphate in new biomineralization media between 36.5 deg. C and 80 deg. C

    Energy Technology Data Exchange (ETDEWEB)

    Temizel, Neslihan; Girisken, Giray; Tas, A. Cuneyt, E-mail: cuneyt-tas@ouhsc.edu

    2011-07-20

    This study investigated the hydrothermal transformation of brushite (dicalcium phosphate dihydrate, DCPD, CaHPO{sub 4}.2H{sub 2}O) into octacalcium phosphate (OCP, Ca{sub 8}(HPO{sub 4}){sub 2}(PO{sub 4}){sub 4}.5H{sub 2}O) in seven different newly developed biomineralization media, all inspired from the commercial DMEM solutions, over the temperature range of 36.5 deg. C to 90 deg. C with aging times varying between 1 h and 6 days. DCPD powders used in this study were synthesized in our laboratory by using a wet-chemical technique. DCPD was found to transform into OCP in the Ca{sup 2+}, Mg{sup 2+}, Na{sup +}, K{sup +}, HCO{sub 3}{sup -}, Cl{sup -} and H{sub 2}PO{sub 4}{sup -} containing aqueous biomineralization media in less than 72 h at 36.5 deg. C, without stirring. The same medium was able to convert DCPD into OCP in about 2 h at 75-80 deg. C, again without a need for stirring. Samples were characterized by using powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). - Research highlights: {yields} New biomineralization solutions developed to convert DCPD into OCP at 36.5 deg. C to 80 deg. C. {yields} DCPD powder was the starting material. {yields} OCP was synthesized under static conditions (no need for stirring). {yields} OCP was synthesized in sealed glass media bottles in solutions free of Hepes or Tris. {yields} OCP can be synthesized at 75-80 deg. C in only 2 hours in the above solutions without stirring.

  7. Dynamical model of brushite precipitation

    Science.gov (United States)

    Oliveira, Cristina; Georgieva, Petia; Rocha, Fernando; Ferreira, António; Feyo de Azevedo, Sebastião

    2007-07-01

    The objectives of this work are twofold. From academic point of view the aim is to build a dynamical macro model to fit the material balance and explain the main kinetic mechanisms that govern the transformation of the hydroxyapatite (HAP) into brushite and the growth of brushite, based on laboratory experiments and collected database. From practical point of view, the aim is to design a reliable process simulator that can be easily imbedded in industrial software for model driven monitoring, optimization and control purposes. Based upon a databank of laboratory measurements of the calcium concentration in solution (on-line) and the particle size distribution (off-line) a reliable dynamical model of the dual nature of brushite particle formation for a range of initial concentrations of the reagents was derived as a system of ordinary differential equations of time. The performance of the model is tested with respect to the predicted evolution of mass of calcium in solution and the average (in mass) particle size along time. Results obtained demonstrate a good agreement between the model time trajectories and the available experimental data for a number of different initial concentrations of reagents.

  8. Nano-sized calcium phosphate (CaP) carriers for non-viral gene deilvery

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Donghyun, E-mail: dhlee@cau.ac.kr [Department of Biomedical Engineering, Division of Integrative Engineering, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul 156-756 (Korea, Republic of); Upadhye, Kalpesh [Department of Bioengineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Kumta, Prashant N., E-mail: pkumta@pitt.edu [Department of Bioengineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Mechanical Engineering and Materials Sceince, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Chemical and Petroleum Engineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Center for Complex Engineered Multifunctional Materials, University of Pittsburgh, Pittsburgh, PA 15261 (United States)

    2012-02-25

    Highlights: Black-Right-Pointing-Pointer Nanostructured calcium phosphates (NanoCaPs): comprehensive review. Black-Right-Pointing-Pointer Non viral gene delivery mechanisms: detailed mechanisms are outlined. Black-Right-Pointing-Pointer Barriers to non-viral gene delivery: detailed barriers are discussed. - Abstract: Gene therapy has garnered much interest due to the potential for curing multiple inherited and/or increases in the acquired diseases. As a result, there has been intense activity from multiple research groups for developing effective delivery methods and carriers, which is a critical step in advancing gene delivery technologies. In order for the carriers to effectively deliver the genetic payloads, multiple extracellular and intracellular barriers need to be overcome. Although overcoming these challenges to improve the effectiveness is critical, the development of safe gene delivery agents is even more vital to assure its use in clinical applications. The development of safe and effective strategies has therefore been a major challenge impeding gene therapy progress. In this regard, calcium phosphate (CaP) based nano-particles has been considered as one of the candidate non-viral gene delivery vehicles, but has been plagued by inconsistent and low transfection efficiencies limiting its progress. There has been major research effort to improve the consistency and effectiveness of CaP based vectors. Currently, it is therefore thought that by controlling the various synthesis factors such as Ca/P ratio, mode of mixing, and type of calcium phosphate phase, such variability and inefficiency could be modulated. This review attempts to provide a comprehensive analysis of the current research activity in the development of CaP based ceramic and polymer-ceramic hybrid systems for non-viral gene delivery. Preliminary transfection results of hydroxyapatite (HA or NanoCaPs), amorphous calcium phosphate (ACP) and brushite phases are also compared to assess the

  9. Role of magnesium on the biomimetic deposition of calcium phosphate

    Science.gov (United States)

    Sarma, Bimal K.; Sarma, Bikash

    2016-10-01

    Biomimetic depositions of calcium phosphate (CaP) are carried out using simulated body fluid (SBF), calcifying solution and newly developed magnesium containing calcifying solution. Calcium phosphate has a rich phase diagram and is well known for its excellent biocompatibility and bioactivity. The most common phase is hydroxyapatite (HAp), an integral component of human bone and tooth, widely used in orthopedic and dental applications. In addition, calcium phosphate nanoparticles show promise for the targeted drug delivery. The doping of calcium phosphate by magnesium, zinc, strontium etc. can change the protein uptake by CaP nanocrystals. This work describes the role of magnesium on the nucleation and growth of CaP on Ti and its oxide substrates. X-ray diffraction studies confirm formation of HAp nanocrystals which closely resemble the structure of bone apatite when grown using SBF and calcifying solution. It has been observed that magnesium plays crucial role in the nucleation and growth of calcium phosphate. A low magnesium level enhances the crystallinity of HAp while higher magnesium content leads to the formation of amorphous calcium phosphate (ACP) phase. Interestingly, the deposition of ACP phase is rapid when magnesium ion concentration in the solution is 40% of calcium plus magnesium ions concentration. Moreover, high magnesium content alters the morphology of CaP films.

  10. Elucidation of real-time hardening mechanisms of two novel high-strength calcium phosphate bone cements.

    Science.gov (United States)

    Smirnov, Valery V; Rau, Julietta V; Generosi, Amanda; Albertini, Valerio Rossi; Ferro, Daniela; Barinov, Sergey M

    2010-04-01

    Despite the numerous literature data available in the field of calcium phosphate bone cements, the mechanism and kinetics of their hardening, both of which are of great importance for cements application, in most cases, is unknown. In this work, the mechanism and kinetics of hardening of two novel high-strength calcium phosphate bone cements were studied using the energy dispersive X-ray diffraction technique, which allows rapid collection of the patterns. The phase transformations occurring on the setting and hardening processes were monitored in situ. Containing minimal quantity of components, whose mixing leads to the formation of cements with pH close to neutral, the cements under study are simple in handling. The main component of both formulations is tetracalcium phosphate. In both cements, the effect of the addition of high- and low-molecular weight chitosan on phase development and kinetics was investigated in detail. One of the cements has the compressive strength of about 70 MPa, whereas the strength of the other, containing Ca(3)Al(2)O(6), is much higher, about 100 MPa. This latter cement could be regarded as an alternative to the common low-strength bioresorbable brushite cements.

  11. Effects of Stirring and Fluid Perfusion on the In Vitro Degradation of Calcium Phosphate Cement/PLGA Composites.

    Science.gov (United States)

    An, Jie; Leeuwenburgh, Sander C G; Wolke, Joop G C; Jansen, John A

    2015-11-01

    In vitro degradation rates of calcium phosphate bioceramics are investigated using a large variation of soaking protocols that do not all match the dynamic conditions of the perfused physiological environment. Therefore, we studied the effect of stirring and fluid perfusion on the in vitro degradation rate of apatitic calcium phosphate cements (CPC) containing poly(lactic-co-glycolic acid) (PLGA) microspheres. The composites were soaked in phosphate-buffered saline up to 6 weeks under unstirred, stirred, or perfused conditions followed by analysis of mass loss, compression strength, porosity, crystal phase composition, and morphology of the cement composites. The results showed that fluid perfusion reduced the decrease in pH and corresponding degradation rates, while nonperfused soaking conditions (i.e., stirred and unstirred conditions) resulted into more extensive acidification, the rate of which increased with stirring. After 2 weeks, the formation of a secondary brushite phase was observed for cement composites soaked under nonperfused (i.e., stirred and unstirred) conditions, whereas this phase was not detected in cements soaked under perfused conditions. The degradation rate of cement composites decreased in the order unstirred>stirred>perfused, as evidenced by quantification of mass loss, compression strength, and pore morphology. To summarize, we have demonstrated that soaking conditions strongly affected the in vitro degradation process of CPCs. As a consequence, it can be concluded that the experimental design of current in vitro degradation studies does not allow for correlation to (pre-)clinical studies.

  12. Biomimetic calcium phosphate coatings on recombinant spider silk fibres

    NARCIS (Netherlands)

    Yang, Liang; Hedhammar, My; Blom, Tobias; Leifer, Klaus; Johansson, Jan; Habibovic, Pamela; Blitterswijk, van Clemens A.

    2010-01-01

    Calcium phosphate ceramic coatings, applied on surfaces of metallic and polymeric biomaterials, can improve their performance in bone repair and regeneration. Spider silk is biocompatible, strong and elastic, and hence an attractive biomaterial for applications in connective tissue repair. Recently,

  13. An Understanding of Renal Stone Development in a Mixed Oxalate–Phosphate System

    OpenAIRE

    2008-01-01

    The in vivo formation of calcium oxalate concretions having calcium phosphate nidi is simulated in an in vitro (37 °C, pH 6.0) dual constant composition (DCC) system undersaturated (σDCPD = −0.330) with respect to brushite (DCPD, CaHPO4 · 2H2O) and slightly supersaturated (σCOM = 0.328) with respect to calcium oxalate monohydrate (COM, CaC2O4 · H2O). The brushite dissolution provides calcium ions that raise the COM supersaturation, which is heterogeneously nucleated either on or near the surf...

  14. Effect of humic substances on the precipitation of calcium phosphate

    Institute of Scientific and Technical Information of China (English)

    SONG Yong-hui; Hermann H. HAHN; Erhard HOFFMANN; Peter G. WEIDLER

    2006-01-01

    For phosphorus (P) recovery from wastewater, the effect of humic substances (HS) on the precipitation of calcium phosphate was studied. Batch experiments of calcium phosphate precipitation were undertaken with synthetic water that contained 20 mg/L phosphate (as P) and 20 mg/L HS (as dissolved organic carbon, DOC) at a constant pH value in the range of 8.0-10.0. The concentration variations of phosphate, calcium (Ca) and HS were measured in the precipitation process; the crystalline state and compositions of the precipitates were analysed by powder X-ray diffraction (XRD) and chemical methods, respectively. It showed that at solution pH 8.0, the precipitation rate and removal efficiency of phosphate were greatly reduced by HS, but at solution pH ≥9.0,the effect of HS was very small. The Ca consumption for the precipitation of phosphate increased when HS was added; HS was also removed from solution with the precipitation of calcium phosphate. At solution pH 8.0 and HS concentrations ≤ 3.5 mg/L, and at pH ≥ 9.0 and HS concentrations ≤ 10 mg/L, the final precipitates were proved to be hydroxyapatite (HAP) by XRD. The increases of solution pH value and initial Ca/P ratio helped reduce the influence of HS on the precipitation of phosphate.

  15. Morphology control of brushite prepared by aqueous solution synthesis

    Directory of Open Access Journals (Sweden)

    T. Toshima

    2014-03-01

    Full Text Available Dicalcium phosphate dihydrate (DCPD, CaHPO4·2H2O, also known as brushite, is one of the important bioceramics due to not only diseases factors such as kidney stone and plaque formation but also purpose as fluoride insolubilization material. It is used medicinally to supply calcium, and is of interest for its unique properties in biological and pathological mineralization. It is important to control the crystal morphology of brushite since its chemical reactivity depends strongly on its surface properties; thus, its morphology is a key issue for its applications as a functional material or precursor for other bioceramics. Here, we report the effects of the initial pH and the Ca and phosphate ion concentrations on the morphology of DCPD particles during aqueous solution synthesis. Crystal morphologies were analyzed by scanning electron microscopy and X-ray diffraction. The morphology phase diagram of DCPD crystallization revealed that increasing the initial pH and/or ion concentration transformed DCPD morphology from petal-like into plate-like structures.

  16. Calcium phosphate precipitation modeling in a pellet reactor

    OpenAIRE

    Montastruc, Ludovic; Azzaro-Pantel, Catherine; Cabassud, Michel; Biscans, Béatrice

    2002-01-01

    The calcium phosphate precipitation in a pellet reactor can be evaluated by two main parameters: the phosphate conversion ratio and the phosphate removal efficiency. The conversion ratio depends mainly on the pH. The pellet reactor efficiency depends not only on pH but also on the hydrodynamical conditions. An efficiency model based on a thermochemical precipitation approach and an orthokinetic aggregation model is presented. In this paper, the results show that optimal conditions for pellet ...

  17. Unique roles of acidic amino acids in phase transformation of calcium phosphates.

    Science.gov (United States)

    Chu, Xiaobin; Jiang, Wenge; Zhang, Zhisen; Yan, Yang; Pan, Haihua; Xu, Xurong; Tang, Ruikang

    2011-02-10

    Although phase transformation is suggested as a key step in biomineralization, the chemical scenario about how organic molecules mediate inorganic phase transformations is still unclear. The inhibitory effect of amino acids on hydroxyapatite (HAP, the main inorganic component of biological hard tissues such as bone and enamel) formation was concluded by the previous biomimetic modeling based upon direct solution crystallization. Here we demonstrate that acidic amino acids, Asp and Glu, could promote HAP crystallization from its precursor crystal, brushite (DCPD). However, such a promotion effect could not be observed when the nonacidic amino acids were applied in the transformation-based HAP formation. We found that the specific modification of acidic amino acid on crystal-solution interfaces played a key role in the phase transition. The distinct properties between DCPD and HAP in the solution resulted in an interfacial energy barrier to suppress the spontaneous formation of HAP phase on DCPD phase. Different from the other amino acids, the carboxylate-rich amino acids, Asp and Glu, could modify the interfacial characteristics of these two calcium phosphate crystals to make them similar to each other. The experiments confirmed that the involvement of Asp or Glu reduced the interfacial energy barrier between DCPD and HAP, leading to a trigger effect on the phase transformation. An in-depth understanding about the unique roles of acidic amino acids may contribute to understanding phase transformation controls druing biomineralization.

  18. Bioactivity and corrosion properties of gelatin-containing and strontium-doped calcium phosphate composite coating

    Science.gov (United States)

    Huang, Yong; Yan, Yajing; Pang, Xiaofeng; Ding, Qiongqiong; Han, Shuguang

    2013-10-01

    To improve coating corrosion resistance and bioactivity, strontium (Sr) and gelatin (GLT) were simultaneously incorporated in calcium phosphate (Ca-P) to form Sr-Ca-P/GLT composite coating on titanium (Ti) by electrodeposition. The surface morphology, chemical composition, phase identification, bond strength, corrosion resistance, and cytocompatibility of the films were studied. Results revealed that the Sr-Ca-P/GLT layer was rough and inhomogeneous, with floral-like crystals or flake agglomerate morphology. The Sr-Ca-P crystals were Sr-doped apatite (hydroxyapatite and brushite), and Sr2+ ions and GLT were homogeneously distributed in the Ca-P coating. The thickness of the composite coating was almost 10 μm without delamination and/or cracking at the interface. The bond strength of the composite coating was 5.6 ± 1.8 MPa. The Sr-Ca-P/GLT coated Ti had lower corrosion rates than bare Ti, suggesting a protective character of the composite coating. Osteoblast cellular tests demonstrated that the Sr-Ca-P/GLT composite coating better enhanced the in vitro biocompatibility of Ti than Ca-P coating.

  19. Bioactivity and corrosion properties of gelatin-containing and strontium-doped calcium phosphate composite coating

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Yong [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); College of Lab Medicine, Hebei North University, Zhangjiakou 075000 (China); Yan, Yajing [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); Pang, Xiaofeng, E-mail: pxf2012@yahoo.com.cn [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China); International Centre for Materials Physics, Chinese Academy of Science, Shenyang 110015 (China); Ding, Qiongqiong; Han, Shuguang [Institute of Life Science and Technology, University of Electronic Science and Technology of China, Chengdu 610054 (China)

    2013-10-01

    To improve coating corrosion resistance and bioactivity, strontium (Sr) and gelatin (GLT) were simultaneously incorporated in calcium phosphate (Ca–P) to form Sr–Ca–P/GLT composite coating on titanium (Ti) by electrodeposition. The surface morphology, chemical composition, phase identification, bond strength, corrosion resistance, and cytocompatibility of the films were studied. Results revealed that the Sr–Ca–P/GLT layer was rough and inhomogeneous, with floral-like crystals or flake agglomerate morphology. The Sr–Ca–P crystals were Sr-doped apatite (hydroxyapatite and brushite), and Sr{sup 2+} ions and GLT were homogeneously distributed in the Ca–P coating. The thickness of the composite coating was almost 10 μm without delamination and/or cracking at the interface. The bond strength of the composite coating was 5.6 ± 1.8 MPa. The Sr–Ca–P/GLT coated Ti had lower corrosion rates than bare Ti, suggesting a protective character of the composite coating. Osteoblast cellular tests demonstrated that the Sr–Ca–P/GLT composite coating better enhanced the in vitro biocompatibility of Ti than Ca–P coating.

  20. The system CaHPO 4·2H 2O-CaSO 4·2H 2O: crystallizations from calcium phosphate solutions in the presence of SO 2-4

    Science.gov (United States)

    Rinaudo, C.; Lanfranco, A. M.; Franchini-Angela, M.

    1994-09-01

    The crystallization from solutions of 36 × 10 -3M in [Ca] 2- = [HPO 4] 2-, with ratios [SO 4] 2-/[HPO 4] 2- ranging from 0.11 to 1, was studied at 25°C. When [SO 4] 2- was present in the starting solutions in small amounts (ratios 0.11-0.43), only brushite, twinned following the [010] direction, crystallized. The morphology and habit of the crystals were strongly dependent on the supersaturation of the solution. Higher concentrations in [SO 4] 2- (ratios 0.66-1) allowed the crystallization, on the brushite first precipitated, of a phase showing, by EDS and X-ray analyses, a calcium sulphate phosphate hydrate composition.

  1. Associations between calcium-phosphate metabolism and coronary artery calcification

    DEFF Research Database (Denmark)

    Grønhøj, Mette H; Gerke, Oke; Mickley, Hans;

    2016-01-01

    calcium-phosphate metabolism is associated with the presence and extent of coronary artery calcification (CAC) in asymptomatic and apparently healthy individuals. METHODS: Serum samples from 1088 randomly recruited middle-aged men and women without known CVD and diabetes (DM), from the general population......, were analysed for total calcium, phosphate, parathyroid hormone (PTH) and 25-hydroxyvitamin D (25(OH)D). CAC was measured by a non-contrast cardiac CT scan and categorised into four groups: 0, 1-99, 100-399, ≥400 Agatston units. The association of calcium-phosphate metabolism with CAC was evaluated......)D values were placed within the normal range. In men, the odds of being in a higher CAC category, i.e. having more severe CAC, increased by 30% when serum calcium concentration increased by 0.1 mmol/l (95% CI: 1.04-1.61, p = 0.019), independently of traditional cardiovascular risk factors. In women...

  2. An X-ray absorption method for the identification of calcium phosphate species using peak height ratios

    Science.gov (United States)

    Oxmann, J. F.

    2013-11-01

    X-ray absorption near edge structure (XANES) studies on calcium phosphate species (Ca-P) deal with marginal differences among subtle spectral features despite a hitherto missing systematic breakdown of these differences. Related fingerprinting approaches depend therefore on spectral libraries that are not validated against each other, incomplete and scattered among publications. This study compiled a comprehensive spectral library from published reference compound libraries in order to establish more clear-cut criteria for Ca-P determination by distinctive phosphorus K-edge XANES features. A specifically developed normalization method identified diagnostic spectral features within the compiled library, e.g. by uniform calculation of ratios between white-line and secondary peak heights. Post-processing of the spectra (n = 81) verified distinguishability among most but not all phases, which included hydroxylapatite (HAP), poorly crystalline HAP, amorphous HAP, fluorapatite, carbonate fluorapatite (CFAP), carbonate hydroxylapatite, β-tricalcium phosphate, octacalcium phosphate (OCP), brushite, monetite, monocalcium phosphate, amorphous calcium phosphate (ACP), anapaite, herderite, scholzite, messelite, whiteite and P on CaCO3. Particularly, peak height ratios significantly improved analyte specificity, e.g. by supplementary breakdown into OCP and ACP. The spectral analysis also revealed Ca-P standards that were rarely investigated or inappropriately synthesized, and thus provides a basis for standard selection and synthesis. The developed method and resulting breakdown by species were subsequently tested on Ca-P spectra from studies on bone and sediment. The test indicated that bone material likely comprises only poorly crystalline apatite, which implies direct nucleation of apatite in bone. This biological apatite formation is likely opposed to that of sedimentary apatite, which apparently forms by successive crystallization. Application of the method to

  3. Technical Note: An X-ray absorption method for the identification of calcium phosphate species using peak-height ratios

    Science.gov (United States)

    Oxmann, J. F.

    2014-04-01

    X-ray absorption near edge structure (XANES) studies on calcium phosphate species (Ca-P) deal with marginal differences among subtle spectral features despite a hitherto missing systematic breakdown of these differences. Related fingerprinting approaches depend, therefore, on spectral libraries that are not validated against each other, incomplete and scattered among publications. This study compiled a comprehensive spectral library from published reference compound libraries in order to establish more clear-cut criteria for Ca-P determination by distinctive phosphorus K-edge XANES features. A specifically developed normalization method identified diagnostic spectral features in the compiled library, e.g. by uniform calculation of ratios between white-line and secondary peak heights. Post-processing of the spectra (n = 81) verified distinguishability among most but not all phases, which included hydroxylapatite (HAP), poorly crystalline HAP, amorphous HAP, fluorapatite, carbonate fluorapatite (CFAP), carbonate hydroxylapatite, β-tricalcium phosphate, octacalcium phosphate (OCP), brushite, monetite, monocalcium phosphate, amorphous calcium phosphate (ACP), anapaite, herderite, scholzite, messelite, whiteite and P on CaCO3. Particularly, peak-height ratios significantly improved analyte specificity, e.g. by supplementary breakdown into OCP and ACP. The spectral analysis also revealed Ca-P standards that were rarely investigated or inappropriately synthesized, and thus provides a basis for standard selection and synthesis. The method developed and resulting breakdown by species were subsequently tested on Ca-P spectra from studies on bone and sediment. The test indicated that bone material likely comprises only poorly crystalline apatite, which confirms direct nucleation of apatite in bone. This biological apatite formation is likely opposed to that of sedimentary apatite, which apparently forms by both direct nucleation and successive crystallization. Application of

  4. The use of size-defined DNA-functionalized calcium phosphate nanoparticles to minimise intracellular calcium disturbance during transfection.

    Science.gov (United States)

    Neumann, Sebastian; Kovtun, Anna; Dietzel, Irmgard D; Epple, Matthias; Heumann, Rolf

    2009-12-01

    Calcium phosphate-based transfection methods are frequently used to transfer DNA into living cells. However, it has so far not been studied in detail to what extend the different transfection methods lead to a net calcium uptake. Upon subsequent resolution of the calcium phosphate, intracellular free ionic calcium-surges could result, inducing as side effect various physiological responses that may finally result in cell death. Here we investigated the overall calcium uptake by the human bladder carcinoma cell line T24 during the standard calcium phosphate transfection method and also during transfection with custom-made calcium phosphate/DNA nanoparticles by isotope labelling with (45)calcium. (45)Calcium uptake was strongly increased after 7h of standard calcium phosphate transfection but not if the transfection was performed with calcium phosphate nanoparticles. Time lapse imaging microscopy using the calcium-sensitive dye Fura-2 revealed large transient increases of the intracellular free calcium level during the standard calcium phosphate transfection but not if calcium phosphate nanoparticles were used. Consistently, the viability of cells transfected by calcium phosphate/DNA nanoparticles was not changed, in remarkable contrast to the standard method where considerable cell death occurred.

  5. Calcium phosphate bioceramics prepared from wet chemically precipitated powders

    Directory of Open Access Journals (Sweden)

    Kristine Salma

    2010-03-01

    Full Text Available In this work calcium phosphates were synthesized by modified wet chemical precipitation route. Contrary to the conventional chemical precipitation route calcium hydroxide was homogenized with planetary mill. Milling calcium oxide and water in planetary ball mill as a first step of synthesis provides a highly dispersed calcium hydroxide suspension. The aim of this work was to study the influence of main processing parameters of wet chemical precipitation synthesis product and to control the morphology, phase and functional group composition and, consequently, thermal stability and microstructure of calcium phosphate bioceramics after thermal treatment. The results showed that it is possible to obtain calcium phosphates with different and reproducible phase compositions after thermal processing (hydroxyapatite [HAp], β-tricalcium phosphate [β-TCP] and HAp/β-TCP by modified wet-chemical precipitation route. The β-TCP phase content in sintered bioceramics samples is found to be highly dependent on the changes in technological parameters and it can be controlled with ending pH, synthesis temperature and thermal treatment. Pure, crystalline and highly thermally stable (up to 1300°C HAp bioceramics with homogenous grainy microstructure, grain size up to 200–250 nm and high open porosity can be successfully obtained by powder synthesized at elevated synthesis temperature of 70°C and stabilizing ending pH at 9.

  6. The effect of crystal structure of TiO2 nanotubes on the formation of calcium phosphate coatings during biomimetic deposition

    Science.gov (United States)

    Liu, Yi; Kim, Sun; McLeod, John A.; Li, Jun; Guo, Xiaoxuan; Sham, Tsun-Kong; Liu, Lijia

    2017-02-01

    The crystallization process of bioactive calcium phosphate (CaP) species via biomimetic deposition onto anodic TiO2 nanotubes is investigated. The porous surface of nanostructured TiO2 provides an ideal substrate for CaP crystallization. The compositions of CaP coatings are studied using X-ray absorption near-edge structures (XANES) at the Ca K-edge. Using detection modes with different probing depths, both the surface of the CaP coating and the CaP-TiO2 interface are simultaneously analyzed. Calcium phosphate (CaP) species, such as hydroxyapatite (HAp), octacalcium phosphate (Ca8(HPO4)2(PO4)4·5H2O, OCP), brushite (CaHPO4·2H2O, DCPD), and amorphous calcium phosphate (ACP), are found in the CaP coatings. TiO2 nanotubes of amorphous and anatase phases are comparatively studied to determine their effect on the efficiency of CaP formation and the phase transformation among CaP species in prolonged deposition time. It is found the composition of CaP coating has a strong dependency on the crystal structure of TiO2 substrate and the kinetics (deposition time).

  7. Renal control of calcium, phosphate, and magnesium homeostasis.

    Science.gov (United States)

    Blaine, Judith; Chonchol, Michel; Levi, Moshe

    2015-07-01

    Calcium, phosphate, and magnesium are multivalent cations that are important for many biologic and cellular functions. The kidneys play a central role in the homeostasis of these ions. Gastrointestinal absorption is balanced by renal excretion. When body stores of these ions decline significantly, gastrointestinal absorption, bone resorption, and renal tubular reabsorption increase to normalize their levels. Renal regulation of these ions occurs through glomerular filtration and tubular reabsorption and/or secretion and is therefore an important determinant of plasma ion concentration. Under physiologic conditions, the whole body balance of calcium, phosphate, and magnesium is maintained by fine adjustments of urinary excretion to equal the net intake. This review discusses how calcium, phosphate, and magnesium are handled by the kidneys.

  8. Effect of proteins and their conformation change during brushite transformation to hydroxyapatite

    Science.gov (United States)

    Xie, Jing

    2000-10-01

    Hydroxyapatite (HA, Ca5(PO4)3OH) coatings on metallic orthopedic implant are being used to achieve implant integration. However, HA is stable in physiological solutions, other more reactive calcium phosphate ceramics (CPC) such as brushite (CaHPO4·2H 2O) have been found to release calcium and phosphate ions during their transformation to HA. The release of these ions may induce faster bone growth and enhance implant integration. This work examines the biocompatibility of the CPC phases that form during the transformation process. Since biocompatibility is associated with cellular response, which in turn is initiated by protein adsorption, this work focuses on the mutual effect between protein adsorption and CPC transformation. The first part of the study is focused on the influence of protein adsorption on transformation kinetics and chemistry. Brushite coated samples immersed in protein free and proteinaceous physiological solutions were retrieved after different exposures times. These were examined using XRD, EDS and FTIR/reflectance. Results show that the presence of Bovine Serum Albumin (BSA) in physiological solution retards the transformation, but the presence of Fibronectin (FN) accelerates the transformation to HA. Interestingly, neither BSA nor FN alters the transformation chemistry. Due to the limitations of the techniques used, this part of the work does not monitor the effect of transformation on adsorbed proteins but only the effect of adsorbed protein on the transforming calcium phosphate coating. The second part of the work examines in situ conformational changes of adsorbed proteins during the CPC transformation using FTIR/ATR. Protein adsorbed on different surfaces such as germanium, CPC, zinc selenide and titanium shows different conformation indicated by the Amide I and II absorption bands in the infrared spectra. During the transformation of brushite to HA, both BSA and FN show a continuous change in conformation, which suggests that the

  9. Optimization of calcium phosphate fine ceramic powders preparation

    Science.gov (United States)

    Sezanova, K.; Tepavitcharova, S.; Rabadjieva, D.; Gergulova, R.; Ilieva, R.

    2013-12-01

    The effect of biomimetic synthesis method, reaction medium and further precursor treatments on the chemical and phase composition, crystal size and morphology of calcium phosphates was examined. Nanosized calcium phosphate precursors were biomimetically precipitated by the method of continuous precipitation in three types of reaction media at pH 8: (i) SBF as an inorganic electrolyte system; (ii) organic (glycerine) modified SBF (volume ratio of 1:1); (iii) polymer (10 g/l xanthan gum or 10 g/l guar gum) modified SBF (volume ratio of 1:1). After maturation (24 h) the samples were lyophilized, calcinated at 300°C for 3 hours, and washed with water, followed by new gelation, lyophilization and step-wise (200, 400, 600, 800, and 1000°C, each for 3 hours) sintering. The reaction medium influenced the chemical composition and particle size but not the morphology of the calcium phosphate powders. In all studied cases bi-phase calcium phosphate fine powders with well-shaped spherical grains, consisting of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) with a Ca/P ratio of 1.3 - 1.6 were obtained. The SBF modifiers decreased the particle size of the product in the sequence guar gum ˜ xanthan gum < glycerin < SBF medium.

  10. Rickets induced by calcium or phosphate depletion.

    OpenAIRE

    Abugassa, S.; Svensson, O.

    1990-01-01

    We studied the effects of calciopenia and phosphopenia on longitudinal growth, skeletal mineralization, and development of rickets in young Sprague-Dawley rats. At an age of 21 days, two experimental groups were given diets containing 0.02% calcium or 0.02% phosphorus; otherwise the diets were nutritionally adequate. After 7, 14, and 21 days, five animals from each group were randomly chosen. The animals were anaesthetized and blood samples were drawn for analysis of calcium, phosphorus, and ...

  11. Thermal reactions of brushite cements.

    Science.gov (United States)

    Bohner, M; Gbureck, U

    2008-02-01

    The thermal reactions of a brushite cement made of beta-tricalcium phosphate (beta-TCP), monocalcium phosphate monohydrate (MCPM), and an aqueous solution were followed in situ with an isothermal calorimeter at 37 degrees C. The investigated parameters were the beta-TCP/MCPM weight ratio, the liquid-to-powder ratio, the synthesis route and milling duration of the beta-TCP powder, as well as the presence of sulfate, citrate, and pyrophosphate ions in the mixing liquid. The thermograms were complex, particularly for mixtures containing an excess of MCPM or additives in the mixing solution. Results suggested that the endothermic MCPM dissolution and the highly exothermic beta-TCP dissolution occurred simultaneously, thereby leading to the formation of a large exothermic peak at early reaction time. Both reactions were followed by the exothermic crystallization of brushite and in the presence of an excess of MCPM by the endothermic crystallization of monetite. Additives generally widened the main exothermic reaction peak, or in some cases with pyrophosphate ions postponed the main exothermic peak at late reaction time. Generally, the results could be well explained and understood based on thermodynamic and solubility data.

  12. Study of in vitro degradation of brushite cements scaffolds.

    Science.gov (United States)

    de Oliveira Renó, Caroline; Pereta, Nicholas C; Bertran, Celso A; Motisuke, Mariana; de Sousa, Eliandra

    2014-10-01

    An interest path to fabricate supports for tissue engineering is to foam calcium phosphate cement's pastes leading to an increase on material's total porosity and interconnectivity which facilitates cells' adhesion, proliferation and differentiation. The aim of this work is to develop scaffolds of brushite cement and to evaluate its in vitro degradation rate. Macroporosity was obtained by foaming the liquid phase with different non-ionic surfactants (Tween 80 and Lutensol ON-110). The foam stability was achieved by adding chitosan. The scaffolds were immersed in Ringers(®) solution during 7, 14, 21 and 28 days and samples' microstructure, weight loss, mechanical resistance and apparent porosity were evaluated. Both scaffolds presented interconnected macropores with sizes ranging from 100 to 360 µm and total porosities higher than 60%. These properties could facilitate cell infiltration, bone growth and vascularization. The scaffolds obtained in this work should be considered as promising materials for application in bone tissue engineering.

  13. Hydrolytic conversion of amorphous calcium phosphate into apatite accompanied by sustained calcium and orthophosphate ions release.

    Science.gov (United States)

    Niu, Xufeng; Chen, Siqian; Tian, Feng; Wang, Lizhen; Feng, Qingling; Fan, Yubo

    2017-01-01

    The aim of this study is to investigate the calcium and orthophosphate ions release during the transformation of amorphous calcium phosphate (ACP) to hydroxyapatite (HA) in aqueous solution. The ACP is prepared by a wet chemical method and further immersed in the distilled water for various time points till 14d. The release of calcium and orthophosphate ions is measured with calcium and phosphate colorimetric assay kits, respectively. The transition of ACP towards HA is detected by x-ray diffraction (XRD), transmission electron microscopy (TEM), and fourier transform infrared spectroscopy (FTIR). The results indicate that the morphological conversion of ACP to HA occurs within the first 9h, whereas the calcium and orthophosphate ions releases last for over 7d. Such sustained calcium and orthophosphate ions release is very useful for ACP as a candidate material for hard tissue regeneration.

  14. Enhanced mechanical properties of a novel, injectable, fiber-reinforced brushite cement.

    Science.gov (United States)

    Maenz, Stefan; Kunisch, Elke; Mühlstädt, Mike; Böhm, Anne; Kopsch, Victoria; Bossert, Jörg; Kinne, Raimund W; Jandt, Klaus D

    2014-11-01

    Injectable, brushite-forming calcium phosphate cements (CPCs) have great potential as bone replacement materials due to enhanced degradability and long-term inclusion in bone remodeling. However, the use of such brushite-forming CPCs in load-bearing areas is limited by their low mechanical strength. One approach to overcome this limitation is the use of reinforcing fibers. Thus, an injectable, biodegradable, brushite-forming CPC based on beta-tricalcium phosphate/phosphoric acid with fiber reinforcement was developed for minimally invasive surgery. The fibers (diameter 25 µm; length 0.25, 1 or 2mm) were extruded from poly(l-lactide-co-glycolide) acid (PLGA) and added to the CPC (2.5, 5 or 7.5% (w/w)). Independent of the fiber content, injectability of the CPC was retained up to a fiber length of 1mm. The addition of all PLGA fiber types increased diametral tensile strength, biaxial flexural strength, and flexural strength by up to 25% (p ≤ 0.05 for the diametral tensile strength for the CPC with 5% (w/w) 1mm fibers and the biaxial flexural strength of the CPC with 5% (w/w) 0.25 mm fibers). In contrast, the work of fracture strongly and significantly increased (pfiber content, the mechanical properties of the fiber-reinforced CPC were mostly augmented with increasing fiber length. Also, the addition of PLGA fibers to the brushite-forming CPC (up to 7.5% (w/w)) only transiently delayed cell growth and did not decrease cell viability. Fiber reinforcement of CPCs thus augments their mechanical strength while preserving the injectability and biocompatibility required for their application in modern surgery.

  15. Morphometric immunohistochemical examination of the inflammatory tissue reaction after implantation of calcium phosphate-coated titanium plates in rats.

    Science.gov (United States)

    Walschus, Uwe; Hoene, Andreas; Neumann, Hans-Georg; Wilhelm, Lutz; Lucke, Silke; Lüthen, Frank; Rychly, Joachim; Schlosser, Michael

    2009-02-01

    Calcium phosphate (CaP) preparations are established coatings for titanium-based medical implants used for bone reconstruction. However, biodegradation of the coating can result in microparticles that subsequently cause inflammatory reactions. The present study was therefore aimed at investigating the inflammatory response to two series of CaP-coated titanium plates: Ti-brushite (Ti-B) and Ti-hydroxyapatite (Ti-H) implants. Fifteen male LEW.1A rats received one plate of each series and a pellet (5 x 2 mm) of sol-gel derived silica/CaP (SCP implants) implanted into the back musculature. After 7, 14 and 28 days, five rats were killed and the implants were removed with the surrounding tissue. Quantitative immunohistochemistry was performed on frozen sections. Total monocytes/macrophages, tissue macrophages, T-cells, MHC-class-II-positive cells and proliferating cells were counted. For the Ti-B implants, the number of monocytes/macrophages remained constant while the other cell populations increased. In contrast, for the Ti-H implants the number of monocytes/macrophages decreased while the other cell populations remained constant. The SCP implants demonstrated degradation and scattering into smaller particles with an increase for all cell populations except the proliferating cells. Human mesenchymal stem cells demonstrated adherence and a flat morphology on Ti-B and Ti-H implants and no remarkable difference between both implants. Taken together, the in vivo data demonstrate that the short-term inflammatory response against a hydroxyapatite coating is lower in comparison to a brushite coating, and that the morphology of cells growing in vitro is similar on both layers.

  16. Biomimetic calcium phosphate coatings on recombinant spider silk fibres

    Energy Technology Data Exchange (ETDEWEB)

    Yang Liang; Habibovic, Pamela; Van Blitterswijk, Clemens A [Department of Tissue Regeneration, University of Twente, PO Box 217, 7500 AE Enschede (Netherlands); Hedhammar, My; Johansson, Jan [Department of Anatomy, Physiology and Biochemistry, Swedish University of Agricultural Sciences, the Biomedical Centre, Box 575, 751 23 Uppsala (Sweden); Blom, Tobias; Leifer, Klaus [Department of Engineering Sciences, Uppsala University, Box 534, S-751 21 Uppsala (Sweden)

    2010-08-01

    Calcium phosphate ceramic coatings, applied on surfaces of metallic and polymeric biomaterials, can improve their performance in bone repair and regeneration. Spider silk is biocompatible, strong and elastic, and hence an attractive biomaterial for applications in connective tissue repair. Recently, artificial spider silk, with mechanical and structural characteristics similar to those of native spider silk, has been produced from recombinant minispidroins. In the present study, supersaturated simulated body fluid was used to deposit calcium phosphate coatings on recombinant spider silk fibres. The mineralization process was followed in time using scanning electron microscopy equipped with an energy dispersive x-ray (EDX) detector and Raman spectroscope. Focused ion beam technology was used to produce a cross section of a coated fibre, which was further analysed by EDX. Preliminary in vitro experiments using a culture of bone marrow-derived human mesenchymal stem cells (hMSCs) on coated fibres were also performed. This study showed that recombinant spider silk fibres were successfully coated with a homogeneous and thick crystalline calcium phosphate layer. In the course of the mineralization process from modified simulated body fluid, sodium chloride crystals were first deposited on the silk surface, followed by the deposition of a calcium phosphate layer. The coated silk fibres supported the attachment and growth of hMSCs.

  17. Microporous calcium phosphate ceramics driving osteogenesis through surface architecture

    NARCIS (Netherlands)

    Zhang, J.; Barbieri, D.; Hoopen, ten H.W.M.; Bruijn, de J.D.; Blitterswijk, van C.A.; Yuan, H.

    2015-01-01

    The presence of micropores in calcium phosphate (CaP) ceramics has shown its important role in initiating inductive bone formation in ectopic sites. To investigate how microporous CaP ceramics trigger osteoinduction, we optimized two biphasic CaP ceramics (i.e., BCP-R and BCP-S) to have the same che

  18. lectrolytic deposition of lithium into calcium phosphate coatings

    NARCIS (Netherlands)

    Wang, Jiawei; Groot, de Klaas; Blitterswijk, van Clemens; Boer, de Jan

    2009-01-01

    Objectives: Lithium ions stimulate the Wnt signaling pathway and the authors previously demonstrated that lithium enhances the proliferation of tissue cultured human mesenchymal stem cells. The aim of this study was to prepare and characterize a calcium phosphate/lithium coating by means of electrol

  19. Atomic structure of intracellular amorphous calcium phosphate deposits.

    Science.gov (United States)

    Betts, F; Blumenthal, N C; Posner, A S; Becker, G L; Lehninger, A L

    1975-06-01

    The radial distribution function calculated from x-ray diffraction of mineralized cytoplasmic structures isolated from the hepatopancreas of the blue crab (Callinectes sapidus) is very similar to that previously found for synthetic amorphous calcium phosphate. Both types of mineral apparently have only short-range atomic order, represented as a neutral ion cluster of about 10 A in longest dimension, whose probable composition is expressed by the formula Ca9(PO4)6. The minor differences observed are attributed to the presence in the biological mineral of significant amounts of Mg-2+ and ATP. Synthetic amorphous calcium phosphate in contact with a solution containing an amount of ATP equivalent to that of the biological mineral failed to undergo conversion to the thermodynamically more stable hydroxyapatite. The amorphous calcium phosphate of the cytoplasmic mineral granules is similarly stable, and does not undergo conversion to hydroxyapatite, presumably owing to the presence of ATP and Mg-2+, known in inhibitors of the conversion process. The physiological implications of mineral deposits consisting of stabilized calcium phosphate ion clusters are discussed.

  20. Calcium phosphate implants coatings as carriers for BMP-2

    NARCIS (Netherlands)

    Liu, Y.; He, J.F.; Hunziker, E.B.

    2009-01-01

    The osteoconductivity of dental implants can be improved by coating them with a layer of calcium phosphate (CaP), which can be rendered osteoinductive by functionalizing it with an osteogenic agent, such as bone morphogenetic protein 2 (BMP-2). In the present study, we wished to compare the osteoind

  1. Pathogenic role of basic calcium phosphate crystals in destructive arthropathies

    NARCIS (Netherlands)

    Ea, H.K.; Chobaz, V.; Nguyen, C.; Nasi, S.; Lent, P.L. van; Daudon, M.; Dessombz, A.; Bazin, D.; McCarthy, G.; Jolles-Haeberli, B.; Ives, A.; Linthoudt, D. Van; So, A.; Liote, F.; Busso, N.

    2013-01-01

    BACKGROUND: basic calcium phosphate (BCP) crystals are commonly found in osteoarthritis (OA) and are associated with cartilage destruction. BCP crystals induce in vitro catabolic responses with the production of metalloproteases and inflammatory cytokines such as interleukin-1 (IL-1). In vivo, IL-1

  2. Injectable calcium phosphate cement for bone repair and implant fixation.

    NARCIS (Netherlands)

    Jansen, J.; Ooms, E.M.; Verdonschot, N.J.J.; Wolke, J.G.C.

    2005-01-01

    The studies as described are aimed at determining the efficacy of newly developed calcium phosphate cement when this material is used as a bone defect filler or gap filler around metal implants. An overview is provided about bone graft substitutes and methods of metal implant fixation.

  3. Mechanical properties of porous, electrosprayed calcium phosphate coatings

    NARCIS (Netherlands)

    Leeuwenburgh, S.C.G.; Wolke, J.G.C.; Lommen, L.; Pooters, T.; Schoonman, J.; Jansen, J.A.

    2006-01-01

    Mechanical properties of calcium phosphate coatings (CaP), deposited using the electrostatic spray deposition (ESD) technique, have been characterized using a range of analytical techniques, including tensile testing (ASTM C633), fatigue testing (ASTM E855), and scratch testing using blunt and sharp

  4. Synthesis of Brushite Particles in Reverse Microemulsions of the Biosurfactant Surfactin

    Directory of Open Access Journals (Sweden)

    Young-Fo Chang

    2011-06-01

    Full Text Available In this study the “green chemistry” use of the biosurfactant surfactin for the synthesis of calcium phosphate using the reverse microemulsion technique was demonstrated. Calcium phosphates are bioactive materials that are a major constituent of human teeth and bone tissue. A reverse microemulsion technique with surfactin was used to produce nanocrystalline brushite particles. Structural diversity (analyzed by SEM and TEM resulted from different water to surfactin ratios (W/S; 250, 500, 1000 and 40,000. The particle sizes were found to be in the 16–200 nm range. Morphological variety was observed in the as-synthesized microemulsions, which consisted of nanospheres (~16 nm in diameter and needle-like (8–14 nm in diameter and 80–100 nm in length noncalcinated particles. However, the calcinated products included nanospheres (50–200 nm in diameter, oval (~300 nm in diameter and nanorod (200–400 nm in length particles. FTIR and XRD analysis confirmed the formation of brushite nanoparticles in the as-synthesized products, while calcium pyrophosphate was produced after calcination. These results indicate that the reverse microemulsion technique using surfactin is a green process suitable for the synthesis of nanoparticles.

  5. Synthesis of brushite particles in reverse microemulsions of the biosurfactant surfactin.

    Science.gov (United States)

    Maity, Jyoti Prakash; Lin, Tz-Jiun; Cheng, Henry Pai-Heng; Chen, Chien-Yen; Reddy, A Satyanarayana; Atla, Shashi B; Chang, Young-Fo; Chen, Hau-Ren; Chen, Chien-Cheng

    2011-01-01

    In this study the "green chemistry" use of the biosurfactant surfactin for the synthesis of calcium phosphate using the reverse microemulsion technique was demonstrated. Calcium phosphates are bioactive materials that are a major constituent of human teeth and bone tissue. A reverse microemulsion technique with surfactin was used to produce nanocrystalline brushite particles. Structural diversity (analyzed by SEM and TEM) resulted from different water to surfactin ratios (W/S; 250, 500, 1000 and 40,000). The particle sizes were found to be in the 16-200 nm range. Morphological variety was observed in the as-synthesized microemulsions, which consisted of nanospheres (~16 nm in diameter) and needle-like (8-14 nm in diameter and 80-100 nm in length) noncalcinated particles. However, the calcinated products included nanospheres (50-200 nm in diameter), oval (~300 nm in diameter) and nanorod (200-400 nm in length) particles. FTIR and XRD analysis confirmed the formation of brushite nanoparticles in the as-synthesized products, while calcium pyrophosphate was produced after calcination. These results indicate that the reverse microemulsion technique using surfactin is a green process suitable for the synthesis of nanoparticles.

  6. Biologically Analogous Calcium Phosphate Tubes from a Chemical Garden.

    Science.gov (United States)

    Hughes, Erik A B; Williams, Richard L; Cox, Sophie C; Grover, Liam M

    2017-02-28

    Calcium phosphate (CaPO4) tubes with features comparable to mineralized biological microstructures, such as Haversian canals, were grown from a calcium gel/phosphate solution chemical garden system. A significant difference in gel mass in response to high and low solute phosphate equivalent environments existed within 30 min of solution layering upon gel (p = 0.0067), suggesting that the nature of advective movement between gel and solution is dependent on the solution concentration. The transport of calcium cations (Ca(2+)) and phosphate anions (PO4(3-)) was quantified and changes in pH were monitored to explain the preferential formation of tubes within a PO4(3-) concentration range of 0.5-1.25 M. Ingress from the anionic solution phase into the gel followed by the liberation of Ca(2+) ions from the gel was found to be essential for acquiring self-assembled tubular CaPO4 structures. Tube analysis by scanning electron microscopy (SEM), X-ray diffraction (XRD), and micro X-ray florescence (μ-XRF) revealed hydroxyapatite (HA, Ca10(PO4)6(OH)2) and dicalcium phosphate dihydrate (DCPD, CaHPO4·2H2O) phases organized in a hierarchical manner. Notably, the tubule diameters ranged from 100 to 150 μm, an ideal size for the permeation of vasculature in biological hard tissue.

  7. Amorphous calcium phosphate and its application in dentistry

    Directory of Open Access Journals (Sweden)

    Sun Wei-bin

    2011-07-01

    Full Text Available Abstract Amorphous Calcium Phosphate (ACP is an essential mineral phase formed in mineralized tissues and the first commercial product as artificial hydroxyapatite. ACP is unique among all forms of calcium phosphates in that it lacks long-range, periodic atomic scale order of crystalline calcium phosphates. The X-ray diffraction pattern is broad and diffuse with a maximum at 25 degree 2 theta, and no other different features compared with well-crystallized hydroxyapatite. Under electron microscopy, its morphological form is shown as small spheroidal particles in the scale of tenths nanometer. In aqueous media, ACP is easily transformed into crystalline phases such as octacalcium phosphate and apatite due to the growing of microcrystalline. It has been demonstrated that ACP has better osteoconductivity and biodegradability than tricalcium phosphate and hydroxyapatite in vivo. Moreover, it can increase alkaline phosphatase activities of mesoblasts, enhance cell proliferation and promote cell adhesion. The unique role of ACP during the formation of mineralized tissues makes it a promising candidate material for tissue repair and regeneration. ACP may also be a potential remineralizing agent in dental applications. Recently developed ACP-filled bioactive composites are believed to be effective anti-demineralizing/remineralizing agents for the preservation and repair of tooth structures. This review provides an overview of the development, structure, chemical composition, morphological characterization, phase transformation and biomedical application of ACP in dentistry.

  8. Calcium-phosphate-osteopontin particles for caries control

    DEFF Research Database (Denmark)

    Schlafer, Sebastian

    Oftentimes caries lesions develop in protected sites that are difficult to access by self-performed mechanical tooth cleaning. At present, there is a growing interest in chemical adjuncts to mechanical procedures of oral hygiene that aim at biofilm control rather than biofilm eradication. Calcium......-phosphate-osteopontin particles are a new promising therapeutic approach to caries control. They are designed to bind to dental biofilms and interfere with biofilm build-up, lowering the bacterial burden on the tooth surface without affecting bacterial viability in the oral cavity. Moreover, they dissolve when pH in the biofilm...... drops to 6 or below and release buffering phosphate ions that stabilize biofilm pH above the critical level for enamel dissolution. With that twofold approach, calcium-phosphate-osteopontin particles may make a relevant contribution to clinical caries control....

  9. Calcium-phosphate-osteopontin particles for caries control

    DEFF Research Database (Denmark)

    Schlafer, Sebastian; Birkedal, Henrik; Olsen, Jakob

    2016-01-01

    Caries is caused by acid production in biofilms on dental surfaces. Preventing caries therefore involves control of microorganisms and/or the acid produced. Here, calcium-phosphate-osteopontin particles are presented as a new approach to caries control. The particles are made by co......-precipitation and designed to bind to bacteria in biofilms, impede biofilm build-up without killing the microflora, and release phosphate ions to buffer bacterial acid production if the pH decreases below 6. Analysis of biofilm formation and pH in a five-species biofilm model for dental caries showed that treatment......H always remained above 5.5. Hence, calcium-phosphate-osteopontin particles show potential for applications in caries control....

  10. Formation of calcium phosphate mineral materialcontrolled by microemulsion

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    In order to prepare calcium phosphate-based material with nano-structure and bioactivity, natural lecithin and n-tetradecane were used as the amphipile and the oil phase respectively, along with the water phase, to form a microemulsion template. Phosphate mineralization was induced and controlled by the microemulsion. The products, characterized by scanning electronic microscopy, infrared spectroscopy and X-ray diffraction analysis, are composed of lecithin and hydroxyapatite, and possess the nano-structure of sticks, balls and three-dimensional nets connected by tubes. These results show that the microemulsion can be used to control calcium phosphate mineralization for the preparation of biomimetic mineral materials with various nano-structures.

  11. Fibre-reinforced calcium phosphate cements: a review.

    Science.gov (United States)

    Canal, C; Ginebra, M P

    2011-11-01

    Calcium phosphate cements (CPC) consist of one or more calcium orthophosphate powders, which upon mixing with water or an aqueous solution, form a paste that is able to set and harden after being implanted within the body. Different issues remain still to be improved in CPC, such as their mechanical properties to more closely mimic those of natural bone, or their macroporosity to favour osteointegration of the artificial grafts. To this end, blends of CPC with polymer and ceramic fibres in different forms have been investigated. The present work aims at providing an overview of the different approaches taken and identifying the most significant achievements in the field of fibre-reinforced calcium phosphate cements for clinical applications, with special focus on their mechanical properties.

  12. Synthesis and characterization of powders calcium phosphate for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, D.M.P. de; Prants, W.T.; Camargo, N.H.A.; Gemelli, E., E-mail: daniellapinheiro@gmail.com, E-mail: w_prants@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: dma2ec@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas

    2009-07-01

    Scientists of different areas research the bioceramics as new materials to substitute parts of the human body. The bioceramics of the calcium phosphate have the advantage present similar chemical composition to the structure of the bony apatite of the human skeleton. In this study, calcium phosphate powder was synthesized chemically using the solution of phosphorus pentoxide (P{sub 2}O{sub 5}) and calcium oxide (CaO) necessary for molar Ca/P =1.67. These works aim the study of different thermal treatments, physics and of the microstructure properties. For characterization the bony matrix were used the techniques of: X-ray diffraction (DRX); Scanning Electronic Microscopy (SEM) and Differential Scanning Calorimetry (DSC). (author)

  13. Degradation processes of reinforced concretes by combined sulfate–phosphate attack

    Energy Technology Data Exchange (ETDEWEB)

    Secco, Michele, E-mail: michele.secco@unipd.it [Inter-Departmental Research Center for the Study of Cement Materials and Hydraulic Binders (CIRCe), University of Padova, Via Gradenigo 6, 35131 Padova (Italy); Department of Civil, Environmental and Architectural Engineering (ICEA), University of Padova, Via Marzolo 9, 35131 Padova (Italy); Lampronti, Giulio Isacco, E-mail: gil21@cam.ac.uk [Department of Earth Sciences, University of Cambridge, Downing Street, CB2 3EQ Cambridge (United Kingdom); Schlegel, Moritz-Caspar, E-mail: moritz-caspar.schlegel@helmholtz-berlin.de [BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, 12205 Berlin (Germany); Helmholtz-Zentrum Berlin fürMaterialien und Energie GmbH, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Maritan, Lara, E-mail: lara.maritan@unipd.it [Department of Geosciences, University of Padova, Via Gradenigo 6, 35131 Padova (Italy); Zorzi, Federico, E-mail: federico.zorzi@unipd.it [Department of Geosciences, University of Padova, Via Gradenigo 6, 35131 Padova (Italy)

    2015-02-15

    A novel form of alteration due to the interaction between hydrated cement phases and sulfate and phosphate-based pollutants is described, through the characterization of concrete samples from an industrial reinforced concrete building. Decalcification of the cement matrices was observed, with secondary sulfate and phosphate-based mineral formation, according to a marked mineralogical and textural zoning. Five alteration layers may be detected: the two outermost layers are characterized by the presence of gypsum–brushite solid solution phases associated with anhydrous calcium sulfates and phosphates, respectively, while a progressive increase in apatite and ammonium magnesium phosphates is observable in the three innermost layers, associated with specific apatite precursors (brushite, octacalcium phosphate and amorphous calcium phosphate, respectively). The heterogeneous microstructural development of secondary phases is related to the chemical, pH and thermal gradients in the attacked cementitious systems, caused by different sources of pollutants and the exposure to the sun's radiation.

  14. Conversion of Marine Structures to Calcium Phosphate Materials: Mechanisms of Conversion Using Two Different Phosphate Solutions

    OpenAIRE

    Macha, Innocent J.; Grossin, David; Ben-Nissan, Besim

    2016-01-01

    International audience; Marine structure, coralline materials were converted to calcium phosphate using twodifferent phosphate solutions. The aim was to study the conversion mechanisms under acidic andbasic environment at moderate conditions of temperature. Crystal growth and morphology ofconverted corals were characterized by XRD and SEM respectively. The results suggested thatunder acidic conditions (H3PO4), dissolution and precipitation control and direct the crystalformation and morpholog...

  15. (31)P Solid-State NMR study of the chemical setting process of a dual-paste injectable brushite cements.

    Science.gov (United States)

    Legrand, A P; Sfihi, H; Lequeux, N; Lemaître, J

    2009-10-01

    The composition and evolution of a brushite-type calcium phosphate cement was investigated by Solid-State NMR and X-ray during the setting process. The cement is obtained by mixing beta-tricalcium phosphate [Ca(3)(PO(4))(2), beta-TCP] and monocalcium phosphate monohydrate [Ca(H(2)PO(4))(2).H(2)O, MCPM] in presence of water, with formation of dicalcium phosphate dihydrate or brushite [CaHPO(2).2H(2)O, DCPD]. Analysis of the initial beta-TCP paste has shown the presence of beta-calcium pyrophosphate [Ca(2)P(2)O(7), beta-CPy] and that of the initial MCPM a mixture of MCPM and dicalcium phosphate [CaHPO(4), DCP]. Follow-up of the chemical composition by (31)P Solid-State NMR enables to show that the chemical setting process appeared to reach an end after 20 min. The constant composition observed at the end of the process was similarly determined.

  16. In vivo behavior of a novel injectable calcium phosphate cement compared with two other commercially available calcium phosphate cements.

    NARCIS (Netherlands)

    Hannink, G.; Wolke, J.G.C.; Schreurs, B.W.; Buma, P.

    2008-01-01

    The aim of this study was to investigate the physicochemical and biological properties of a newly developed calcium phosphate cement (CPC). The novel cement was compared with two other commercially available CPCs. After mixing the powder and liquid phase, the CPCs were injected as a paste into a rab

  17. The relationship between the morphology of brushite crystals grown rapidly in silica gel and its structure

    Science.gov (United States)

    Ohta, M.; Tsutsumi, M.

    1982-02-01

    The morphology of brushite, CaHPO 4 · 2 H 2O, provides some basic information on biological mineralization. The growth, morphology and surface structures of brushite crystals grown at fairly high growth rates in silica gel at 37°C in the initial pH range of 4 to 6 (the final pH range of about 3.2 to 4.7) have been investigated. Their preferred growth direction is [101]: there is a marked tendency for calcium and phosphate ions in the gel to attach to (111) or (101) surfaces; inclusions derived from silica gel are also incorporated, mainly along the [101] direction in the initial stage of crystal growth and at higher pH values. The following order of "edge strength", which refers to a sort of resistance of crystal edge against getting out of its shape, was obtained experimentally for the edges parallel to the (010) face of brushite: [101] ⪆ [201] > [001] ⪆ [100]. The relationship between the above order and the structure of corrugated sheets with composition [CaHPO 4] is also discussed.

  18. High-strength resorbable brushite bone cement with controlled drug-releasing capabilities.

    Science.gov (United States)

    Hofmann, M P; Mohammed, A R; Perrie, Y; Gbureck, U; Barralet, J E

    2009-01-01

    Brushite cements differ from apatite-forming compositions by consuming a lot of water in their setting reaction whereas apatite-forming cements consume little or no water at all. Only such cement systems that consume water during setting can theoretically produce near-zero porosity ceramics. This study aimed to produce such a brushite ceramic and investigated whether near elimination of porosity would prevent a burst release profile of incorporated antibiotics that is common to prior calcium phosphate cement delivery matrices. Through adjustment of the powder technological properties of the powder reactants, that is particle size and particle size distribution, and by adjusting citric acid concentration of the liquid phase to 800mM, a relative porosity of as low as 11% of the brushite cement matrix could be achieved (a 60% reduction compared to previous studies), resulting in a wet unprecompacted compressive strength of 52MPa (representing a more than 100% increase to previously reported results) with a workable setting time of 4.5min of the cement paste. Up to 2wt.% of vancomycin and ciprofloxacin could be incorporated into the cement system without loss of wet compressive strength. It was found that drug release rates could be controlled by the adjustable relative porosity of the cement system and burst release could be minimized and an almost linear release achieved, but the solubility of the antibiotic (vancomycin>ciprofloxacin) appeared also to be a crucial factor.

  19. Calcium phosphate/porous silicon biocomposites prepared by cyclic deposition methods: spin coating vs electrochemical activation.

    Science.gov (United States)

    Hernandez-Montelongo, J; Gallach, D; Naveas, N; Torres-Costa, V; Climent-Font, A; García-Ruiz, J P; Manso-Silvan, M

    2014-01-01

    Porous silicon (PSi) provides an excellent platform for bioengineering applications due to its biocompatibility, biodegradability, and bioresorbability. However, to promote its application as bone engineering scaffold, deposition of calcium phosphate (CaP) ceramics in its hydroxyapatite (HAP) phase is in progress. In that sense, this work focuses on the synthesis of CaP/PSi composites by means of two different techniques for CaP deposition on PSi: Cyclic Spin Coating (CSC) and Cyclic Electrochemical Activation (CEA). Both techniques CSC and CEA consisted on alternate Ca and P deposition steps on PSi. Each technique produced specific morphologies and CaP phases using the same independent Ca and P stem-solutions at neutral pH and at room temperature. The brushite (BRU) phase was favored with the CSC technique and the hydroxyapatite (HAP) phase was better synthesized using the CEA technique. Analyses by elastic backscattering spectroscopy (EBS) on CaP/PSi structures synthesized by CEA supported that, by controlling the CEA parameters, an HAP coating with the required Ca/P atomic ratio of 1.67 can be promoted. Biocompatibility was evaluated by bone-derived progenitor cells, which grew onto CaP/PSi prepared by CSC technique with a long-shaped actin cytoskeleton. The density of adhered cells was higher on CaP/PSi prepared by CEA, where cells presented a normal morphological appearance and active mitosis. These results can be used for the design and optimization of CaP/PSi composites with enhanced biocompatibility for bone-tissue engineering.

  20. Influence of calcium on ceramide-1-phosphate monolayers

    Directory of Open Access Journals (Sweden)

    Joana S. L. Oliveira

    2016-02-01

    Full Text Available Ceramide-1-phosphate (C1P plays an important role in several biological processes, being identified as a key regulator of many protein functions. For instance, it acts as a mediator of inflammatory responses. The mediation of the inflammation process happens due to the interaction of C1P with the C2 domain of cPLA2α, an effector protein that needs the presence of submicromolar concentrations of calcium ions. The aim of this study was to determine the phase behaviour and structural properties of C1P in the presence and absence of millimolar quantities of calcium in a well-defined pH environment. For that purpose, we used monomolecular films of C1P at the soft air/liquid interface with calcium ions in the subphase. The pH was varied to change the protonation degree of the C1P head group. We used surface pressure versus molecular area isotherms coupled with other monolayer techniques as Brewster angle microscopy (BAM, infrared reflection–absorption spectroscopy (IRRAS and grazing incidence X-ray diffraction (GIXD. The isotherms indicate that C1P monolayers are in a condensed state in the presence of calcium ions, regardless of the pH. At higher pH without calcium ions, the monolayer is in a liquid-expanded state due to repulsion between the negatively charged phosphate groups of the C1P molecules. When divalent calcium ions are added, they are able to bridge the highly charged phosphate groups, enhancing the regular arrangement of the head groups. Similar solidification of the monolayer structure can be seen in the presence of a 150 times larger concentration of monovalent sodium ions. Therefore, calcium ions have clearly a strong affinity for the phosphomonoester of C1P.

  1. The different phases in the precipitation of dicalcium phosphate dihydrate

    Science.gov (United States)

    Ferreira, A.; Oliveira, C.; Rocha, F.

    2003-05-01

    The precipitation of dicalcium phosphate dihydrate, brushite, by mixing a calcium hydroxide suspension and an orthophosphoric acid solution in equimolar quantities, has been investigated in a batch system at 25°C. The concentration of calcium hydroxide and orthophosphoric acid, before mixing, ranged from 50 to 300 mmol dm -3. The phase first precipitated is Ca 5OH(PO 4) 3, hydroxyapatite. The precipitation process of brushite is divided into five stages and is similar for all initial experimental conditions. The extension of each stage varies with the initial reagents' concentrations. These stages are discussed individually as a function of pH and reagents' concentrations. The precipitate was analysed by scanning electron microscopy and X-ray diffraction. The solubility of brushite was determined at 25°C, 30°C and 35°C, and in the pH range 4.5-8.

  2. Diagnosis and clinical manifestations of calcium pyrophosphate and basic calcium phosphate crystal deposition diseases.

    Science.gov (United States)

    Ea, Hang-Korng; Lioté, Frédéric

    2014-05-01

    Basic calcium phosphate and pyrophosphate calcium crystals are the 2 main calcium-containing crystals that can deposit in all skeletal tissues. These calcium crystals give rise to numerous manifestations, including acute inflammatory attacks that can mimic alarming and threatening differential diagnoses, osteoarthritis-like lesions, destructive arthropathies, and calcific tendinitis. Awareness of uncommon localizations and manifestations such as intraspinal deposition (eg, crowned dens syndrome, tendinitis of longus colli muscle, massive cervical myelopathy compression) prevents inappropriate procedures and cares. Coupling plain radiography, ultrasonography, computed tomography, and synovial fluid analysis allow accurate diagnosis by directly or indirectly identifying the GRAAL of microcrystal-related symptoms.

  3. Hybrid Calcium Phosphate Coatings for Titanium Implants

    Science.gov (United States)

    Kharapudchenko, E.; Ignatov, V.; Ivanov, V.; Tverdokhlebov, S.

    2017-01-01

    Hybrid multilayer coatings were obtained on titanium substrates by the combination of two methods: the micro-arc oxidation in phosphoric acid solution with the addition of calcium compounds to high supersaturated state and RF magnetron sputtering of the target made of synthetic hydroxyapatite. 16 different groups of coatings were formed on titanium substrates and in vitro studies were conducted in accordance with ISO 23317 in the solution simulating body fluid. The studies using SEM, XRD of the coatings of the samples before and after exposure to SBF were performed. The features of morphology, chemical and phase composition of the studied coatings are shown.

  4. Urinary stone formation: Efficacy of seed extract of Ensete superbum (Roxb.) Cheesman on growth inhibition of calcium hydrogen phosphate dihydrate crystals

    Science.gov (United States)

    Diana, K. J.; George, K. V.

    2013-01-01

    The effect of aqueous seed extract of Ensete superbum (Roxb.) Cheesman on in vitro crystallization and growth patterns of calcium hydrogen phosphate dihydrate (CaHPO4·2H2O, CHPD) crystals was studied using single diffusion gel growth technique. Reduction in growth of CHPD crystals was noticed with increasing concentrations of seed extract. The morphology of CHPD or brushite crystals was studied by microscopy. The structural changes of the treated crystals were assessed by SEM, FT-IR, XRD and TGA/DTA analysis. It is expected that this multidisciplinary approach for in vitro crystallization and characterization of CHPD crystals will provide a better explanation to develop novel strategies for prevention of urinary stones.

  5. Mechanism of calcium phosphates precipitation in liquid crystals; Mecanisme de precipitation de phosphates de calcium dans des cristaux liquides

    Energy Technology Data Exchange (ETDEWEB)

    Prelot, B.; Zemb, T

    2004-04-01

    The possibility of using as a precursor an easily wet meso-porous powder would be a breakthrough in the preparation of nuclear waste storage ceramics. A concentrated solution containing ions to be stored would wet a dry powder and then, subjected to mild compression, lead to a micro-crystalline matrix of calcium phosphate at acceptable temperatures. Since no porous calcium phosphate different from calcined bone (patented) is described as porous precursor, we have compared the different synthesis routes towards meso-porous ceramics. First, we considered homogeneous precipitation of slats in water: using initially off-stoichiometry in reaction, micron-sized hydroxyapatite particles are produced with a specific surface up to 100 m{sup 2}/g. Then, we consider the classical route of precipitation of an hybrid material in the miscibility gap of a phase diagram, when an hexagonal liquid crystal is used a matrix for precipitation. The surfactant family consists in single chain surfactants containing phosphates as head-group to poison the growing surface of calcium phosphate nano-domains. Since the reaction is still too brutal, we considered using a cat-anionic precursor material of controllable surface charge. For certain concentrations and molar ratios, a new structure not yet described in surfactant precipitation literature is observed: since the periodicity is lower than twice the chain length, a disordered constant curvature monolayer (instead of the classical cylinder of twice chain length diameter) of surfactant is implied. Finally, we have investigated synthesis routes implying slow dissolution of pre-formed calcium phosphate in an already existing hexagonal matrix. For all these routes of synthesis, micro-structural determinations using SAXS, WARS and BET are performed, with a special attention to comparison of the precipitation material, the matrix obtained with all elements present, and also the material obtained after calcinations. (authors)

  6. Tetracalcium phosphate: Synthesis, properties and biomedical applications.

    Science.gov (United States)

    Moseke, C; Gbureck, U

    2010-10-01

    Monoclinic tetracalcium phosphate (TTCP, Ca(4)(PO(4))(2)O), also known by the mineral name hilgenstockite, is formed in the (CaO-P(2)O(5)) system at temperatures>1300 degrees C. TTCP is the only calcium phosphate with a Ca/P ratio greater than hydroxyapatite (HA). It appears as a by-product in plasma-sprayed HA coatings and shows moderate reactivity and concurrent solubility when combined with acidic calcium phosphates such as dicalcium phosphate anhydrous (DCPA, monetite) or dicalcium phosphate dihydrate (DCPD, brushite). Therefore it is widely used in self-setting calcium phosphate bone cements, which form HA under physiological conditions. This paper aims to review the synthesis and properties of TTCP in biomaterials applications such as cements, sintered ceramics and coatings on implant metals.

  7. Effect of carbon fiber on calcium phosphate bone cement

    Institute of Scientific and Technical Information of China (English)

    戴红莲; 王欣宇; 黄健; 闫玉华; 李世普

    2004-01-01

    The calcium phosphate cement (α-TCP/TTCP) was reinforced with oxidation-treated carbon fibers. The effect of aspect ratio and content of carbon fiber on the compression strength and bending strength of the hardened body was discussed. The results show that the reinforcing effect is optimal as the aspect ratio is 375 and the additive amount is 0.3% (mass fraction). Under this condition, the compressive strength is increased by 55% (maximum 63.46 MPa), and the bending strength is nearly increased by 100% (maximum 11.95 MPa), respectively. However, if the additive quantity and aspect ratio are too high, the effect of the carbon fibers is limited because it can not be dispersed uniformly in the hardened body. The biological evaluation indicates that the calcium phosphate cement reinforced by carbon fibers has good biocompatibility.

  8. Advantages of using glycolic acid as a retardant in a brushite forming cement.

    Science.gov (United States)

    Mariño, Faleh Tamimi; Torres, Jesús; Hamdan, Mohammad; Rodríguez, Carmen Rueda; Cabarcos, Enrique López

    2007-11-01

    In this study we have compared the effect of using acetic, glycolic, and citric acids on the brushite cement setting reaction and the properties of the resultant cement. The cement solid phase was made by mixing beta-tricalcium phosphate (beta-TCP), monocalcium dihydrogen phosphate anhydrate (MCPA), and sodium pyrophosphate, whereas the cement liquid phase consisted of aqueous solutions of carboxy acids at concentrations ranging from 0.5 to 3.5M. Cements were prepared by mixing the solid phase with the liquid phase to form a workable paste. The cement setting time was longer for glycolic and citric acids. The best mechanical properties in dry environments were obtained using glycolic and citric acid liquid phases. In a wet environment at 37 degrees C, the cement set with glycolic acid was the strongest one. Brushite cement diametral tensile strength seems to be affected by the calcium-carboxyl phase produced in the setting reaction. The acceptable setting time and mechanical properties of cements set in glycolic acid solutions are attributed to the additional hydrophilic groups in the carboxylic acid and the low solubility in water of the calcium salt produced in the reaction. Moreover, at high concentrations, carboxylic acids add chemically to the cement matrix becoming reactants themselves.

  9. Calcium Phosphate Coating over Silk Fibroin Film by Biomimetic Methods

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    To investigate the biomineralization behavior of silk fibroin and to valuate the biodegradation and biocompatibility of the hybrid biomaterial, the calcium phosphate deposits were identified with SEM, EDX,XRD and FTIR. The results reveal that supersaturated calcification solution is an effective method for the mineralization of fibroin film. Enzymatic degradation experiment demonstrates the biodegradability of the composites. Osteoblasts incubation shows an excellent cytocompatibility on the mineralized fibroin films.

  10. Bone tissue incorporates in vitro gallium with a local structure similar to gallium-doped brushite.

    Science.gov (United States)

    Korbas, M; Rokita, E; Meyer-Klaucke, W; Ryczek, J

    2004-01-01

    During mineral growth in rat bone-marrow stromal cell cultures, gallium follows calcium pathways. The dominant phase of the cell culture mineral constitutes the poorly crystalline hydroxyapatite (HAP). This model system mimics bone mineralization in vivo. The structural characterization of the Ga environment was performed by X-ray absorption spectroscopy at the Ga K-edge. These data were compared with Ga-doped synthetic compounds (poorly crystalline hydroxyapatite, amorphous calcium phosphate and brushite) and with strontium-treated bone tissue, obtained from the same culture model. It was found that Sr(2+) substitutes for Ca(2+) in the HAP crystal lattice. In contrast, the replacement by Ga(3+) yielded a much more disordered local environment of the probe atom in all investigated cell culture samples. The coordination of Ga ions in the cell culture minerals was similar to that of Ga(3+), substituted for Ca(2+), in the Ga-doped synthetic brushite (Ga-DCPD). The Ga atoms in the Ga-DCPD were coordinated by four oxygen atoms (1.90 A) of the four phosphate groups and two oxygen atoms at 2.02 A. Interestingly, the local environment of Ga in the cell culture minerals was not dependent on the onset of Ga treatment, the Ga concentration in the medium or the age of the mineral. Thus, it was concluded that Ga ions were incorporated into the precursor phase to the HAP mineral. Substitution for Ca(2+ )with Ga(3+) distorted locally this brushite-like environment, which prevented the transformation of the initially deposited phase into the poorly crystalline HAP.

  11. Aggregation of Calcium Phosphate and Oxalate Phases in the Formation of Renal Stones

    OpenAIRE

    2014-01-01

    The majority of human kidney stones are comprised of multiple calcium oxalate monohydrate (COM) crystals encasing a calcium phosphate nucleus. The physiochemical mechanism of nephrolithiasis has not been well determined on the molecular level; this is crucial to the control and prevention of renal stone formation. This work investigates the role of phosphate ions on the formation of calcium oxalate stones; recent work has identified amorphous calcium phosphate (ACP) as a rapidly forming initi...

  12. In vitro studies of calcium phosphate silicate bone cements.

    Science.gov (United States)

    Zhou, Shuxin; Ma, Jingzhi; Shen, Ya; Haapasalo, Markus; Ruse, N Dorin; Yang, Quanzu; Troczynski, Tom

    2013-02-01

    A novel calcium phosphate silicate bone cement (CPSC) was synthesized in a process, in which nanocomposite forms in situ between calcium silicate hydrate (C-S-H) gel and hydroxyapatite (HAP). The cement powder consists of tricalcium silicate (C(3)S) and calcium phosphate monobasic (CPM). During cement setting, C(3)S hydrates to produce C-S-H and calcium hydroxide (CH); CPM reacts with the CH to precipitate HAP in situ within C-S-H. This process, largely removing CH from the set cement, enhances its biocompatibility and bioactivity. The testing results of cell culture confirmed that the biocompatibility of CPSC was improved as compared to pure C(3)S. The results of XRD and SEM characterizations showed that CPSC paste induced formation of HAP layer after immersion in simulated body fluid for 7 days, suggesting that CPSC was bioactive in vitro. CPSC cement, which has good biocompatibility and low/no cytotoxicity, could be a promising candidate as biomedical cement.

  13. An understanding of renal stone development in a mixed oxalate-phosphate system.

    Science.gov (United States)

    Guan, Xiangying; Wang, Lijun; Dosen, Anja; Tang, Ruikang; Giese, Rossman F; Giocondi, Jennifer L; Orme, Christine A; Hoyer, John R; Nancollas, George H

    2008-07-15

    The in vivo formation of calcium oxalate concretions having calcium phosphate nidi is simulated in an in vitro (37 degrees C, pH 6.0) dual constant composition (DCC) system undersaturated (sigma DCPD = -0.330) with respect to brushite (DCPD, CaHPO 4 . 2H 2O) and slightly supersaturated (sigma COM = 0.328) with respect to calcium oxalate monohydrate (COM, CaC2O4 . H2O). The brushite dissolution provides calcium ions that raise the COM supersaturation, which is heterogeneously nucleated either on or near the surface of the dissolving calcium phosphate crystals. The COM crystallites may then aggregate, simulating kidney stone formation. Interestingly, two intermediate phases, anhydrous dicalcium phosphate (monetite, CaHPO4) and calcium oxalate trihydrate (COT), are also detected by X-ray diffraction during this brushite-COM transformation. In support of clinical observations, the results of these studies demonstrate the participation of calcium phosphate phases in COM crystallization providing a possible physical chemical mechanism for kidney stone formation.

  14. Fabrication and characterization of calcium phosphate cement scaffolds; Obtencao e caracterizacao de scaffolds de cimento de fosfato de calcio

    Energy Technology Data Exchange (ETDEWEB)

    Sousa, E. de; Motisuke, M., E-mail: eliandra.sousa@unifesp.br [Universidade Federal de Sao Paulo (UNIFESP), Sao Jose dos Campos, SP (Brazil). Instituto de Ciencia e Tecnologia; Bertran, C.A. [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Instituto de Quimica

    2011-07-01

    In Tissue Engineering, the need for scaffolds which are capable of guiding the organization, differentiation and growth of cells leading to the formation of new tissues is highly relevant. For the development of new scaffolds focused on bone tissue therapy, calcium phosphate cements (CPC) have great potential, because besides their resorbability, they present morphology and chemical composition similar to the bone mineral phase. Moreover, there are several processing techniques to produce ceramic scaffolds: polymeric sponge replication, incorporation of organic material into the ceramic powder, gelcasting, emulsion, among others. The aim of this work was to obtain CPCs scaffolds by using two techniques, emulsion and gelcasting. The scaffolds were characterized by their physical and mechanical properties and the crystalline phases formed after the setting reaction of cement were determined by X-ray diffraction. The samples obtained by both methods presented porosity between 61-65% and the microstructure consists of nearly spherical pores (d5o = 50-100 μm). The mechanical strength of the samples ranged from 5.5 to 1.5 MPa. The crystalline phases found were monetite (CaHPO{sub 4}) and brushite (CaHPO{sub 4} 2H{sub 2}O). (author)

  15. Effects of calcium phosphate bioceramics on skeletal muscle cells.

    Science.gov (United States)

    Sun, J S; Tsuang, Y H; Yao, C H; Liu, H C; Lin, F H; Hang, Y S

    1997-02-01

    With advances in ceramics technology, calcium phosphate bioceramics have been applied as bone substitutes. The effects of implants on bony tissue have been investigated. The effects upon adjacent skeletal muscles have not been determined. The focus of this work is to elucidate the biological effects of various calcium phosphate bioceramics on skeletal muscles. Four different kinds of powder of calcium phosphate biomaterials including beta-tricalcium phosphate (beta-TCP), hydroxyapatite (HA), beta-dicalcium pyrophosphate (beta-DCP) and sintered beta-dicalcium pyrophosphate (SDCP), were tested by myoblast cell cultures. The results were analyzed by cell count, cell morphology and concentration of transforming growth factor beta 1 (TGF-beta 1) in culture medium. The cell population and TGF-beta 1 concentration of the control sample increased persistently as the time of culture increased. The changes in cell population and TGF-beta 1 concentration in culture medium of the beta-TCP and HA were quite low in the first 3 days of culture, then increased gradually toward the seventh day. The changes in cell population and TGF-beta 1 concentration in culture medium of the silica, beta-DCP, and SDCP were quite similar. They were lower during the first day of culture but increased and reached that of the control medium after 7 days' culture. Most cells on B-TCP and HA diminished in size with radially spread, long pseudopods. We conclude that HA and beta-TCP are thought to have an inhibitory effect on growth of the myoblasts. The HA and beta-TCP may interfere with the repair and regeneration of injured skeletal muscle after orthopedic surgery.

  16. Effect of calcium carbonate on hardening, physicochemical properties, and in vitro degradation of injectable calcium phosphate cements.

    NARCIS (Netherlands)

    Sariibrahimoglu, K.; Leeuwenburgh, S.C.G.; Wolke, J.G.C.; Yubao, L.; Jansen, J.A.

    2012-01-01

    The main disadvantage of apatitic calcium phosphate cements (CPCs) is their slow degradation rate, which limits complete bone regeneration. Carbonate (CO(3)(2)(-)) is the common constituent of bone and it can be used to improve the degradability of the apatitic calcium phosphate ceramics. This study

  17. Calcium phosphate bioceramics induce mineralization modulated by proteins.

    Science.gov (United States)

    Wang, Kefeng; Leng, Yang; Lu, Xiong; Ren, Fuzeng

    2013-08-01

    Proteins play an important role in the process of biomineralization, which is considered the critical process of new bone formation. The calcium phosphate (Ca-P) mineralization happened on hydroxyapatite (HA), β-tricalcium phosphate (β-TCP) and biphasic calcium phosphate (BCP) when proteins presented were investigated systematically. The results reveal that the presence of protein in the revised simulated body fluid (RSBF) did not alter the shape and crystal structure of the precipitated micro-crystals in the Ca-P layer formed on the three types of bioceramics. However, the morphology of the Ca-P precipitates was regulated but the structure of Ca-P crystal was unchanged in vivo. The presence of proteins always inhibits Ca-P mineralization in RSBF and the degree of inhibitory effect is concentration dependent. Furthermore, Protein presence can increase the possibility of HA precipitation in vitro and in vivo. The results obtained in this study can be helpful for better understanding the mechanism of biomineralization induced by the Ca-P bioceramics.

  18. Kinetics of dissolution of calcium phosphate (Ca-P bioceramics

    Directory of Open Access Journals (Sweden)

    Lukas Brazda

    2008-06-01

    Full Text Available Hydroxyapatite (HAp and β-tricalcium phosphate (β-TCP are widely used bioceramics for surgical or dental applications. This paper is dealing with dissolution kinetics of synthetically prepared β-TCP and four types of HAp granules. Two groups of HAp, treated at different temperatures, each of them with two different granule sizes, were tested. Three corrosive solutions with different pH and simulated body fluid (SBF were used for immersing of the samples. Changes in concentrations of calcium and phosphate ions, pH level and weight changes of the samples were observed. It was found that presence of TRIS buffer enhanced dissolution rate of the β-TCP approximately two times. When exposed to SBF solution, calcium phosphate (most probably hydroxyapatite precipitation predominates over β-TCP dissolution. Results from HAp samples dissolution showed some unexpected findings. Neither heat treatment nor HAp particle size made any major differences in dissolution rate of the same mass of each HAp sample.

  19. Characterization of alginate-brushite in-situ hydrogel composites

    Energy Technology Data Exchange (ETDEWEB)

    Dabiri, Seyed Mohammad Hossein [Department of Informatics, Bioengineering, Robotics, and System Engineering, University of Genoa, Genoa (Italy); Lagazzo, Alberto; Barberis, Fabrizio [Department of Civil, Chemical and Environmental Engineering, University of Genoa, Genoa (Italy); Farokhi, Mehdi [National Cell Bank of Iran, Pasteur Institute of Iran, Tehran (Iran, Islamic Republic of); Finochio, Elisabetta [Department of Civil, Chemical and Environmental Engineering, University of Genoa, Genoa (Italy); Pastorino, Laura [Department of Informatics, Bioengineering, Robotics, and System Engineering, University of Genoa, Genoa (Italy)

    2016-10-01

    In the present study alginate-brushite composite hydrogels were in-situ synthetized and characterized with respect to preparation parameters. Specifically, the influence of initial pH value and initial concentration of phosphate precursor on the in-situ fabrication of the composite hydrogel were taken into account. The composite hydrogels were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric (TGA, DTG) and differential thermal analysis (DTA). Finally, the cell viability tests were carried out (MTT) over the incubation time period of 3, 7, and 14 days. The results revealed that the formation and the crystalline stability of brushite were highly dependent on the initial pH value. It was shown that as the pH reached to the value of 6, characteristics peaks of brushite appeared in the FTIR spectra. Besides, the XRD and thermal analysis results were in a good accordance with those of FTIR. In addition, the SEM images demonstrated that the plate like brushite was formed inside the alginate matrix. Also, a considerable impact of pH variation on the biocompatibility of samples was noticed so that the majority of samples especially those prepared in the acidic conditions were toxic. - Highlights: • Alginate-brushite hydrogel composites were obtained through an in-situ process • The brushite crystals started forming at pH value of 6 • The increase in the initial concentration of phosphate precursor resulted in more crystalline structure • Samples prepared at pH value of 8 had the most stable crystalline structure • Brushite crystals promoted the biocompatibility of alginate.

  20. Selective laser sintering of calcium phosphate materials for orthopedic implants

    Science.gov (United States)

    Lee, Goonhee

    Two technologies, Solid Freeform Fabrication (SFF) and bioceramics are combined in this work to prepare bone replacement implants with complex geometry. SFF has emerged as a crucial technique for rapid prototyping in the last decade. Selective Laser Sintering (SLS) is one of the established SFF manufacturing processes that can build three-dimensional objects directly from computer models without part-specific tooling or human intervention. Meanwhile, there have been great efforts to develop implantable materials that can assist in regeneration of bone defects and injuries. However, little attention has been focused in shaping bones from these materials. The main thrust of this research was to develop a process that can combine those two separate efforts. The specific objective of this research is to develop a process that can construct bone replacement material of complex geometry from synthetic calcium phosphate materials by using the SLS process. The achievement of this goal can have a significant impact on the quality of health care in the sense that complete custom-fit bone and tooth structures suitable for implantation can be prepared within 24--48 hours of receipt of geometric information obtained either from patient Computed Tomographic (CT) data, from Computer Aided Design (CAD) software or from other imaging systems such as Magnetic Resonance Imaging (MRI) and Holographic Laser Range Imaging (HLRI). In this research, two different processes have been developed. First is the SLS fabrication of porous bone implants. In this effort, systematic procedures have been established and calcium phosphate implants were successfully fabricated from various sources of geometric information. These efforts include material selection and preparation, SLS process parameter optimization, and development of post-processing techniques within the 48-hour time frame. Post-processing allows accurate control of geometry and of the chemistry of calcium phosphate, as well as

  1. Use of sodium polyaspartate for the removal of hydroxyapatite/brushite deposits from stainless steel tubing

    Energy Technology Data Exchange (ETDEWEB)

    Littlejohn, F.; Saez, A.E.; Grant, C.S. [North Carolina State Univ., Raleigh, NC (United States). Dept. of Chemical Engineering

    1998-07-01

    This research investigates the use of sodium polyaspartate, a nontoxic, biodegradable polycarboxylic sequestrant, for removing calcium phosphate deposit consisting of hydroxyapatite (HAP) and brushite or dicalcium phosphate dihydrate (DCPD) from stainless steel surfaces. Cleaning studies show that the use of sodium polyaspartate under alkaline conditions significantly enhances the removal rates when compared to deionized water. In acidic solutions, sodium polyaspartate concentrations below 300 ppm inhibit removal of HAP/DCPD deposits whereas higher concentrations increase the removal rate. Comparative cleaning studies at alkaline pHs show that sodium polyaspartate cleans the surface at a rate comparable to sodium citrate but slower than in ethylenediaminetetraacetic acid. Supplementary dissolution experiments show that sodium polyaspartate enhances the HAP/DCPD dissolution rate while inhibiting the release of Ca{sup 2+}. On the basis of these findings, the authors have concluded that sodium polyaspartate improves the HAP/DCPD dissolution and cleaning rates by Ca{sup 2+} sequestration.

  2. Injectable biphasic calcium phosphate bioceramic: The HYDROS concept.

    Science.gov (United States)

    Baroth, Serge; Bourges, Xavier; Goyenvalle, Eric; Aguado, Eric; Daculsi, Guy

    2009-01-01

    A new biphasic calcium phosphate ceramic material has been developed in our laboratory. It is composed of 60% of hydroxyapatite and 40% of beta-tricalcium phosphate, based on three granulometries (submicron, round microporous 80-200 mum and macro microporous 0.5-1 mm particles) and hydrated with water leading the formation of a putty filler for bone repair. Biocompatibility and osteogenicity were tested by filling femoral epiphyses critical size bone defect and lumbar muscles in rabbit. After 3, 6 and 12 weeks of implantation, explants were treated for histology. Results revealed the biocompatibility of the material and intensive resorption of the submicron particle fraction followed by important bone ingrowth whereas osteoconduction was provided by the larger particles.

  3. Porous Calcium Phosphate Ceramic Scaffolds for Tissue Engineering

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    This study examined the biological response of two porous calcium phosphate ceramics,hydroxyapatite (HA) and hydroxyapaptite/ β-tricalcium phosphate ( HA / β- TCP ) scaffolds. Three different cell types, a human osteoblastic cell line (HOS), primary human osteoblasts (HOB) and human mesenchymal stem cells (MSCs), were used to examine biocompatibility and osteoinductive capacity. The experimental results showed both materials were highly biocompatible and proliferation was significantly greater on pure HA ( P <0.01 ), with a peak in proliferation at day 7. Protein levels were significantly higher ( P < 0.05) than the control Thermanox ( TMX(tm)) for both test materials. Osteoinduction of MSCs was observed on both test materials,with cells seeded on HA/ β- TCP showing greater alkaline phosphatase activity compared to HA alone, indicating an enhancement in osteoinductive property. Both materials show good potential for use as tissue engineered scaffolds.

  4. The Transformation of Calcium Phosphate Bioceramics in Vivo

    Institute of Scientific and Technical Information of China (English)

    DAI Hong-lian; CAO Xian-ying; LI Xiao-xi; YAN Yu-hua; LI Shi-pu

    2003-01-01

    To study the transformation process of calcium phosphate bioceramic in vivo,biodegradable porous β-tricalcium phosphate ceramics (β-TCP) were used in this experiment. The materials (φ5×8mm) were implanted in the tibia of rabbits. The β-TCP ceramics with bone tissue were retrieved and treated for histology, and then observed by using a scanning electron microscope (SEM) and an electron probe X-ray microanalyzer (EMPA) every month. The results show that β-TCP ceramics bond to bone directly,new bones are forming and maturing with materials continuous degrading,and the materials are nearly replaced by the formed bone finally.Parts of the materials were degraded,absorpted and recrystallized,the others dispersped on the cancellous bone and the Haversian lamella with an irregular arrangement incorporating in bone formation directly by remodeling structure.

  5. Bioactivity of calcium phosphate bioceramic coating fabricated by laser cladding

    Science.gov (United States)

    Zhu, Yizhi; Liu, Qibin; Xu, Peng; Li, Long; Jiang, Haibing; Bai, Yang

    2016-05-01

    There were always strong expectations for suitable biomaterials used for bone regeneration. In this study, to improve the biocompatiblity of titanium alloy, calcium phosphate bioceramic coating was obtained by laser cladding technology. The microstructure, phases, bioactivity, cell differentiation, morphology and resorption lacunae were investigated by optical microscope (OM), x-ray diffraction (XRD), methyl thiazolyl tetrazolium (MTT) assay, tartrate-resistant acid phosphatase (TRAP) staining and scanning electronic microscope (SEM), respectively. The results show that bioceramic coating consists of three layers, which are a substrate, an alloyed layer and a ceramic layer. Bioactive phases of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) were found in ceramic coating. Osteoclast precursors have excellent proliferation on the bioceramic surface. The bioceramics coating could be digested by osteoclasts, which led to the resorption lacunae formed on its surface. It revealed that the gradient bioceramic coating has an excellent bioactivity.

  6. Setting mechanisms of an acidic premixed calcium phosphate cement

    OpenAIRE

    2013-01-01

    Premixed calcium phosphate cements (pCPC), where glycerol is used instead of water as mixing liquid, present better handling characteristics than water-based cements. However, the setting mechanisms of pCPC have not been described thoroughly. The aim of this paper is to increase the understanding of the setting mechanism of pCPC. The investigated cement starts to set when glycerol is exchanged with water via diffusion of glycerol out to the surrounding body fluid and water into the material. ...

  7. New developments in calcium phosphate bone cements: approaching spinal applications

    OpenAIRE

    Vlad, Maria Daniela

    2009-01-01

    La presente tesis doctoral (i.e., “New developments in calcium phosphate bone cements: approaching spinal applications”) aporta nuevos conocimientos en el campo de los cementos óseos de fosfato de calcio (CPBCs) en relación a su aplicación clínica en el campo de la cirugía vertebral mínimamente invasiva. La hipótesis central de esta investigación fue formulada en los siguientes términos: “Los cementos apatíticos pueden ser (si se optimizan) una alternativa mejor (debido a sus propiedades d...

  8. Preparation of DNA/Gold Nanoparticle Encapsulated in Calcium Phosphate

    Directory of Open Access Journals (Sweden)

    Tomoko Ito

    2011-01-01

    Full Text Available Biocompatible DNA/gold nanoparticle complex with a protective calcium phosphate (CaP coating was prepared by incubating DNA/gold nanoparticle complex coated by hyaluronic acid in SBF (simulated body fluid with a Ca concentration above 2 mM. The CaP-coated DNA complex was revealed to have high compatibility with cells and resistance against enzymatic degradation. By immersion in acetate buffer (pH 4.5, the CaP capsule released the contained DNA complex. This CaP capsule including a DNA complex is promising as a sustained-release system of DNA complexes for gene therapy.

  9. Calcium-phosphate-osteopontin particles for caries control

    DEFF Research Database (Denmark)

    Schlafer, Sebastian

    Oftentimes caries lesions develop in protected sites that are difficult to access by self-performed mechanical tooth cleaning. At present, there is a growing interest in chemical adjuncts to mechanical procedures of oral hygiene that aim at biofilm control rather than biofilm eradication. Calcium......-phosphate-osteopontin particles are a new promising therapeutic approach to caries control. They are designed to bind to dental biofilms and interfere with biofilm build-up, lowering the bacterial burden on the tooth surface without affecting bacterial viability in the oral cavity. Moreover, they dissolve when pH in the biofilm...

  10. Increase of the final setting time of brushite cements by using chondroitin 4-sulfate and silica gel.

    Science.gov (United States)

    Tamimi-Mariño, F; Mastio, J; Rueda, C; Blanco, L; López-Cabarcos, E

    2007-06-01

    Chondroitin 4-sulfate (C4S) is a bioactive glycosaminoglycan with inductive properties in bone and tissue regeneration. Dicalcium phosphate dehydrate cements (known as brushite) are biocompatible and resorbable materials used in bone and dental surgery. In this study we analyzed the effect of C4S on the setting of a calcium phosphate cement and the properties of the resulting material. Brushite based cement powder was synthesised by mixing monocalcium phosphate with beta-tricalcium phosphate and sodium pyrophosphate. When the concentration of C4S, in the liquid added to the cement powder, was between 1 and 8% the cement final setting time increases. Furthermore, the cement diametral tensile strength remains unaffected when solutions with concentrations of C4S below 5% were used, but decreases at higher C4S concentrations. Calorimetric analysis showed that the cements prepared with C4S alone and in combination with silica gel have a greater content of hydrated water. We concluded from our study that the addition of small amounts of C4S increases the cement setting time without affecting its diametral tensile strength and at the same time improves the cement's hydrophilicity.

  11. Microporous calcium phosphate ceramics driving osteogenesis through surface architecture.

    Science.gov (United States)

    Zhang, Jingwei; Barbieri, Davide; ten Hoopen, Hetty; de Bruijn, Joost D; van Blitterswijk, Clemens A; Yuan, Huipin

    2015-03-01

    The presence of micropores in calcium phosphate (CaP) ceramics has shown its important role in initiating inductive bone formation in ectopic sites. To investigate how microporous CaP ceramics trigger osteoinduction, we optimized two biphasic CaP ceramics (i.e., BCP-R and BCP-S) to have the same chemical composition, equivalent surface area per volume, comparable protein adsorption, similar ion (i.e., calcium and phosphate) exchange and the same surface mineralization potential, but different surface architecture. In particular, BCP-R had a surface roughness (Ra) of 325.4 ± 58.9 nm while for BCP-S it was 231.6 ± 35.7 nm. Ceramic blocks with crossing or noncrossing channels of 250, 500, 1000, and 2000 µm were implanted in paraspinal muscle of dogs for 12 weeks. The percentage of bone volume in the channels was not affected by the type of pores (i.e., crossing vs. closed) or their size, but it was greatly influenced by the ceramic type (i.e., BCP-R vs. BCP-S). Significantly, more bone was formed in the channels of BCP-R than in those of BCP-S. Since the two CaP ceramics differed only in their surface architecture, the results hereby demonstrate that microporous CaP ceramics may induce ectopic osteogenesis through surface architecture.

  12. Reinforcement Strategies for Load-Bearing Calcium Phosphate Biocements

    Directory of Open Access Journals (Sweden)

    Martha Geffers

    2015-05-01

    Full Text Available Calcium phosphate biocements based on calcium phosphate chemistry are well-established biomaterials for the repair of non-load bearing bone defects due to the brittle nature and low flexural strength of such cements. This article features reinforcement strategies of biocements based on various intrinsic or extrinsic material modifications to improve their strength and toughness. Altering particle size distribution in conjunction with using liquefiers reduces the amount of cement liquid necessary for cement paste preparation. This in turn decreases cement porosity and increases the mechanical performance, but does not change the brittle nature of the cements. The use of fibers may lead to a reinforcement of the matrix with a toughness increase of up to two orders of magnitude, but restricts at the same time cement injection for minimal invasive application techniques. A novel promising approach is the concept of dual-setting cements, in which a second hydrogel phase is simultaneously formed during setting, leading to more ductile cement–hydrogel composites with largely unaffected application properties.

  13. On the development of an apatitic calcium phosphate bone cement

    Indian Academy of Sciences (India)

    Manoj Komath; H K Varma; R Sivakumar

    2000-04-01

    Development of an apatitic calcium phosphate bone cement is reported. 100 Particles of tetracalcium phosphate (TTCP) and dicalcium phosphate dihydrate (DCPD) were mixed in equimolar ratio to form the cement powder. The wetting medium used was distilled water with Na2HPO4 as accelerator to manipulate the setting time. The cement powder, on wetting with the medium, formed a workable putty. The setting times of the putty were measured using a Vicat type apparatus and the compressive strength was determined with a Universal Testing Machine. The nature of the precipitated cement was analyzed through X-ray diffraction (XRD), fourier transform infrared spectrometry (FTIR) and energy dispersive electron microprobe (EDAX). The results showed the phase to be apatitic with a calcium–to–phosphorous ratio close to that of hydroxyapatite. The microstructure analysis using scanning electron microscopy (SEM) showed hydroxyapatite nanocrystallite growth over particulate matrix surface. The structure has an apparent porosity of ∼ 52%. There were no appreciable dimensional or thermal changes during setting. The cement passed the in vitro toxicological screening (cytotoxicity and haemolysis) tests. Optimization of the cement was done by manipulating the accelerator concentration so that the setting time, hardening time and the compressive strength had clinically relevant values.

  14. New agent to treat elevated phosphate levels: magnesium carbonate/calcium carbonate tablets.

    Science.gov (United States)

    Meyer, Caitlin; Cameron, Karen; Battistella, Marisa

    2012-01-01

    In summary, Binaphos CM, a magnesium carbonate/calcium carbonate combination phosphate binder, is marketed for treating elevated phosphate levels in dialysis patients. Although studies using magnesium/calcium carbonate as a phosphate binder are short term with small numbers of patients, this phosphate binder has shown some promising results and may provide clinicians with an alternative for phosphate binding. Using a combination phosphate binder may reduce pill burden and encourage patient compliance. In addition to calcium and phosphate, it is imperative to diligently monitor magnesium levels in patients started on this medication, as magnesium levels may increase with longer duration of use. Additional randomized controlled trials are necessary to evaluate long-term efficacy and safety of this combination phosphate binder.

  15. The increasing of enamel calcium level after casein phosphopeptideamorphous calcium phosphate covering

    Directory of Open Access Journals (Sweden)

    Widyasri Prananingrum

    2012-06-01

    Full Text Available Background: Caries process is characterized by the presence of demineralization. Demineralization is caused by organic acids as a result of carbohydrate substrate fermentation. Remineralization is a natural repair process for non-cavitated lesions. Remineralization occurs if there are Ca2+ and PO43- ions in sufficient quantities. Casein-amorphous calcium phosphate phosphopeptide (CPP-ACP is a paste material containing milk protein (casein, that actually contains minerals, such as calcium and phosphate. The casein ability to stabilize calcium phosphate and enhance mineral solubility and bioavailability confers upon CPP potential to be biological delivery vehicles for calcium and phosphate. Purpose: The aim of this study was to determine the calcium levels in tooth enamel after being covered with CPP-ACP 2 times a day for 3, 14 and 28 days. Methods: Sample were bovine incisors of 3 year old cows divided into 4 groups, namely group I as control group, group II, III and IV as treatment groups covered with CPP-ACP 2 times a day. All of those teeth were then immersed in artificial saliva. Group II was immersed for 3 days, while group III was immersed for 14 days, and group IV was immersed for 28 days. One drop of CPP-ACP was used to cover the entire labial surface of teeth. The measurement of the calcium levels was then conducted by using titration method. All data were analyzed by One- Way ANOVA test with 5% degree of confidence. Results: The results showed significant difference of the calcium levels in tooth enamel of those groups after covered with CPP-ACP 2 times a day for 3, 14 and 28 days (p = 0.001. There is also significant difference of the calcium levels in tooth enamel of those treatment groups and the control group (p = 0.001. Conclusion: The calcium levels of tooth enamel are increased after covered with CPP-ACP 2 times a day for 3, 14 and 28 days.Latar belakang: Proses terjadinya karies gigi ditandai oleh adanya demineralisasi

  16. Calcium phosphate cements: study of the beta-tricalcium phosphate--monocalcium phosphate system.

    Science.gov (United States)

    Mirtchi, A A; Lemaitre, J; Terao, N

    1989-09-01

    The possibility of making cements based on beta-tricalcium phosphate (beta-TCP), a promising bone graft material, was investigated. Upon admixture with water, beta-TCP/monocalcium phosphate monohydrate (MCPM) mixtures were found to set and harden like conventional hydraulic cements. Beta-TCP powders with larger particle size, obtained by sintering at higher temperatures, increased the ultimate strength of the cement. Results show that setting occurs after dissolution of MCPM, as a result of the precipitation of dicalcium phosphate dihydrate (DCPD) in the paste. The ultimate tensile strength of the hardened cement is proportional to the amount of DCPD formed. Upon ageing above 40 degrees C, DCPD transforms progressively into anhydrous dicalcium phosphate (DCP), thereby decreasing the strength. Ageing of the pastes in 100% r.h. results in a decay of the mechanical properties. This can be ascribed to an intergranular dissolution of the beta-TCP aggregates as a result of the pH lowering brought about by the MCPM to DCPD conversion.

  17. Study on the bonding strength between calcium phosphate/chitosan composite coatings and a Mg alloy substrate

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Jie [School of Chemistry Engineering and Technology, Harbin Institute of Technology, Harbin 150001 (China); Pharmacy College, Jiamusi University, Jiamusi 154007 (China); Dai Changsong, E-mail: changsd@hit.edu.cn [School of Chemistry Engineering and Technology, Harbin Institute of Technology, Harbin 150001 (China); Wei Jie [School of Chemistry Engineering and Technology, Harbin Institute of Technology, Harbin 150001 (China); School of Chemistry and Bioengineering, Suzhou Science Technology University, Suzhou 215009 (China); Wen Zhaohui, E-mail: wenzhaohui1968@163.com [Department of Neuro intern, First Affiliated Hospital of Harbin Medical University, Harbin 150001 (China)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer Calcium phosphate/chitosan composite coatings on the MAO-AZ91D alloy were prepared. Black-Right-Pointing-Pointer The bonding force between the coating and the magnesium alloy was optimized. Black-Right-Pointing-Pointer The composite coating slowed down the corrosion rate of magnesium alloy in m-SBF. - Abstract: In order to improve the bonding strength between calcium phosphate/chitosan composite coatings and a micro-arc oxidized (MAO)-AZ91D Mg alloy, different influencing parameters were investigated in the process of electrophoretic deposition (EPD) followed by conversion in a phosphate buffer solution (PBS). Surface morphology and phase constituents of the as-prepared materials were investigated by using X-ray diffractometer (XRD), Fourier-transformed infrared spectrophotometer (FTIR), Raman spectrometer, scanning electron microscope (SEM) with an energy dispersive spectrometer (EDS), and a thermo gravimetric and differential thermal analyzer (TG-DTA). Scratch tests were carried out to study the bonding properties between the coatings and the substrates. In vitro immersion tests were conducted to determine the corrosion behaviors of samples with and without deposit layers through electrochemical experiments. In the EPD process, the acetic acid content in the electrophoresis suspension and the electrophoretic voltage played important roles in improving the bonding properties, while the contents of chitosan (CS) and nano-hydroxyapatite (nHA, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) in the suspension had less significant influences on the mechanical bonding strength. It was observed that the coatings showed the excellent bonding property when an electrophoretic voltage was in a range of 40-110 V with other reagent amounts as follows: acetic acid: 4.5 vol.%, CS {<=} 0.25 g, nHA {<=} 2.0 g in 200 ml of a CS-acetic acid aqueous solution and nHA {<=} 2.5 g in 300 ml of absolute ethanol. The morphology of the composite coating

  18. [Allergy of calcium phosphate cement material following skull reconstruction: a case report].

    Science.gov (United States)

    Mizowaki, Takashi; Miyake, Shigeru; Yoshimoto, Yuji; Matsuura, Yoshitaka; Akiyama, Sou

    2013-04-01

    The paste form of calcium phosphate cement is often used in skull reconstruction because of the biocompatibility and early handling of these cements. Although it had rarely been shown to produce a foreign body reaction, we encountered a patient who experienced an allergic reaction to calcium phosphate cements(Biopex®. A patch test was performed and a positive reaction to magnesium phosphate was obtained. Biopex® contains magnesium phosphate, so we diagnosed this case as allergic reaction. Pathological analysis revealed infiltration of plasmacytes in the bone flap around the calcium phosphate cement. The postoperative course was uneventful 3 years after surgery. Allergy to calcium phosphate cements is rare, but must be considered in differential diagnosis of its side effects.

  19. Coating of calcium phosphate on biometallic materials by electrophoretic deposition

    Institute of Scientific and Technical Information of China (English)

    ZHANG Er-lin; YANG Ke

    2005-01-01

    Although biometallic materials have been used as bone implant materials for a long time, they are still detected as foreign bodies by human immune system. Calcium phosphate coating, especially hydroxyapatite(HA)coating attracts special attention due to its good biocompatibility. Being one of the effective methods used to deposit HA coating onto the metallic implant, the electrophoretic deposition(EPD) was reviewed in detail, including the process of EPD, the advantages and disadvantages, the important processing factors and the microstructure and mechanical properties of the coating. Research results on the processing and the coating show potential application of EPD process to the biomedical materials surface modification. In addition, the nanoparticulate HA coating as a new trend in HA coating was also introduced.

  20. Augmentation of Pedicle Screw Fixation with Calcium Phosphate Cement

    Institute of Scientific and Technical Information of China (English)

    YANG Shu-hua; FU De-hao; LI Jin; XU Wei-hua; YANG Cao; YE Zhe-wei; ZUO Xiao-yan

    2004-01-01

    To determine whether a biodegradable calcium phosphate cement(CPC) provides significant augmentation of pedicle screw fixation or not,an in vitro biomechanical study was carried out to evaluate the biomechanical effect of CPC in the restoration and augmentation of pedicle screw fixation.Axial pullout test and cyclic bending resistance test were employed in the experiment,and polymethylmethacrylate (PMMA) was chosen as control.The results demonstrate that the pullout strengths following CPC restoration and augmentation are 74% greater on an average than those of the control group,but less than those of PMMA restoration group and augmentation group respectively (increased by 126% versus control).In cyclic bending resistance test,the CPC augmented screws are found to withstand a greater number of cycles or greater loading with less displacement before loosening,but the augmentation effect of PMMA is greater than that of CPC.

  1. Passive and active in vitro resorption of calcium and magnesium phosphate cements by osteoclastic cells.

    Science.gov (United States)

    Grossardt, Christian; Ewald, Andrea; Grover, Liam M; Barralet, Jake E; Gbureck, Uwe

    2010-12-01

    Biocements are clinically applied materials for bone replacement in non-load-bearing defects. Depending on their final composition, cements can be either resorbed or remain stable at the implantation site. Degradation can occur by two different mechanisms, by simple dissolution (passive) or after osteoclastic bone remodeling (active). This study investigated both the passive and active in vitro resorption behavior of brushite (CaHPO₄ · 2H₂O), monetite (CaHPO₄), calcium-deficient hydroxyapatite (CDHA; Ca₉(PO₄)₅HPO₄OH), and struvite (MgNH₄PO₄ · 6H₂O) cements. Passive resorption was measured by incubating the cement samples in a cell culture medium, whereas active resorption was determined during the surface culture of multinuclear osteoclastic cells derived from RAW 264.7 macrophages. Osteoclast formation was confirmed by showing tartrate resistant acid phosphatase (TRAP) activity on CDHA, brushite, and monetite surfaces, as well as by measuring calcitonin receptor (CT-R) expression as an osteoclast-specific protein by Western blot analysis for struvite ceramics. An absence of passive degradation and only marginally active degradation of struvite cement was the most degradable with a passive (active) release of 9.26 (2.92) Mg²+ ions and a total weight loss of 4.7% over 13 days of the study.

  2. Regulation of calcium phosphate formation by native amelogenins in vitro.

    Science.gov (United States)

    Kwak, Seo-Young; Kim, Sonia; Yamakoshi, Yasuo; Simmer, James P; Beniash, Elia; Margolis, Henry C

    2014-08-01

    Our previous in vitro studies have shown that recombinant full-length porcine amelogenin rP172 can transiently stabilize amorphous calcium phosphate (ACP) and uniquely guide the formation of well-aligned bundles of hydroxyapatite (HA) crystals, as seen in the secretory stage of amelogenesis. This functional capacity is dependent on the hydrophilic C-terminal domain of full-length amelogenin. However, we have also found that native phosphorylated (single S-16 site) forms of full-length (P173) and C-terminal cleaved (P148) amelogenins can stabilize ACP for > 2 d and prevent HA formation. The present study was carried out to test the hypothesis that, at reduced concentrations, native full-length P173 also has the capacity to guide ordered HA formation. The effect of P148 and P173 concentrations (0.2-2.0 mg/ml) on the rate of spontaneous calcium phosphate precipitation was monitored via changes in solution pH, while mineral phases formed were assessed using TEM. At higher P173 concentrations (1.0-2.0 mg/ml), limited mineral formation occurred and only ACP nanoparticles were observed during a 48 h period. However, at 0.4 mg/ml P173, a predominance of organized bundles of linear, needle-like HA crystals were observed. At 0.2 mg/ml of P173, limited quantities of less organized HA crystals were found. Although P148 similarly stabilized ACP, it did not guide ordered HA formation, like P173. Hence, the establishment of the hierarchical enamel structure during secretory stage amelogenesis may be regulated by the partial removal of full-length amelogenin via MMP20 proteolysis, while predominant amelogenin degradation products, like P148, serve to prevent uncontrolled mineral formation.

  3. Mechanical property and in vitro biocompatibility of brushite cement modified by polyethylene glycol

    Energy Technology Data Exchange (ETDEWEB)

    Roy, Mangal; DeVoe, Ken; Bandyopadhyay, Amit; Bose, Susmita, E-mail: sbose@wsu.edu

    2012-12-01

    Brushite (dicalcium phosphate dihydrate, DCPD) cement, owing to its high solubility in physiological condition and ability to guide new bone formation, is widely used to treat bone defects. In the present study, we have evaluated the effects of poly ethylene glycol (PEG) addition on the setting time, compressive strength and in vitro biocompatibility of brushite cement. The brushite cements were prepared by mixing {beta}-tricalcium phosphate [{beta}-TCP, Ca{sub 3}(PO{sub 4}){sub 2}] and monocalcium phosphate monohydrate [MCPM, Ca(H{sub 2}PO{sub 4}){sub 2} Dot-Operator H{sub 2}O]. PEG was introduced at 2.0 and 5.0 wt% with the liquid. Introduction of PEG resulted in marginal increase in both initial and final setting time, however, significantly affected the compressive strength. Effects of PEG incorporation on in vitro biocompatibility of brushite cements were studied by using human fetal osteoblast cells (hFOB) cells. Field emission scanning electron microscope (FESEM) images and immunohistochemical analysis indicated that pure and PEG incorporated brushite cement facilitates cell adhesion, proliferation and differentiation. Fewer cells expressed vinculin protein with increased PEG content in the cement. Cell proliferation was found to decrease with increased PEG concentration while the cell differentiation increased with PEG content. Our results provide a better understanding of in vitro biocompatibility of PEG added brushite cements that can be used to customize the cement compositions based on application need. - Highlights: Black-Right-Pointing-Pointer Setting time was not altered for brushite cement with PEG addition. Black-Right-Pointing-Pointer hFOB cell proliferation was found to decrease with increased PEG concentration in brushite cement. Black-Right-Pointing-Pointer Enhanced ALP activity was noticed with addition of PEG in brushite cements.

  4. Long-Term In Vitro Degradation of a High-Strength Brushite Cement in Water, PBS, and Serum Solution

    Directory of Open Access Journals (Sweden)

    Ingrid Ajaxon

    2015-01-01

    Full Text Available Bone loss and fractures may call for the use of bone substituting materials, such as calcium phosphate cements (CPCs. CPCs can be degradable, and, to determine their limitations in terms of applications, their mechanical as well as chemical properties need to be evaluated over longer periods of time, under physiological conditions. However, there is lack of data on how the in vitro degradation affects high-strength brushite CPCs over longer periods of time, that is, longer than it takes for a bone fracture to heal. This study aimed at evaluating the long-term in vitro degradation properties of a high-strength brushite CPC in three different solutions: water, phosphate buffered saline, and a serum solution. Microcomputed tomography was used to evaluate the degradation nondestructively, complemented with gravimetric analysis. The compressive strength, chemical composition, and microstructure were also evaluated. Major changes from 10 weeks onwards were seen, in terms of formation of a porous outer layer of octacalcium phosphate on the specimens with a concomitant change in phase composition, increased porosity, decrease in object volume, and mechanical properties. This study illustrates the importance of long-term evaluation of similar cement compositions to be able to predict the material’s physical changes over a relevant time frame.

  5. Long-Term In Vitro Degradation of a High-Strength Brushite Cement in Water, PBS, and Serum Solution.

    Science.gov (United States)

    Ajaxon, Ingrid; Öhman, Caroline; Persson, Cecilia

    2015-01-01

    Bone loss and fractures may call for the use of bone substituting materials, such as calcium phosphate cements (CPCs). CPCs can be degradable, and, to determine their limitations in terms of applications, their mechanical as well as chemical properties need to be evaluated over longer periods of time, under physiological conditions. However, there is lack of data on how the in vitro degradation affects high-strength brushite CPCs over longer periods of time, that is, longer than it takes for a bone fracture to heal. This study aimed at evaluating the long-term in vitro degradation properties of a high-strength brushite CPC in three different solutions: water, phosphate buffered saline, and a serum solution. Microcomputed tomography was used to evaluate the degradation nondestructively, complemented with gravimetric analysis. The compressive strength, chemical composition, and microstructure were also evaluated. Major changes from 10 weeks onwards were seen, in terms of formation of a porous outer layer of octacalcium phosphate on the specimens with a concomitant change in phase composition, increased porosity, decrease in object volume, and mechanical properties. This study illustrates the importance of long-term evaluation of similar cement compositions to be able to predict the material's physical changes over a relevant time frame.

  6. Characterization of a calcium phosphate cement based on alpha-tricalcium phosphate obtained by wet precipitation process

    Energy Technology Data Exchange (ETDEWEB)

    Thurmer, M.B.; Diehl, C.E.; Vieira, R.S.; Coelho, W.T.G.; Santos, L.A., E-mail: monicathurmer@yahoo.com [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Dept. de Engenharia de Materiais

    2012-07-01

    There are several systems of calcium phosphate cements being studied. Those based on alpha-tricalcium phosphate are of particular interest. After setting they produce calcium deficient hydroxyapatite similar to bone like hydroxyapatite. This work aims to obtain alpha-tricalcium phosphate powders by the wet precipitation process, using calcium nitrate and phosphoric acid as reagents. This powder was characterized by infrared spectroscopy, X-ray diffraction and particle size distribution. In order to prepare the calcium phosphate cement, the powder was mixed with an accelerator in an aqueous solution. The mechanical properties of the cement were assessed and it was evaluated by means of apparent density, X-ray diffraction and scanning electron microscopy. The described method produced crystalline alpha-tricalcium phosphate as the major phase. The calcium phosphate cement showed high values of compression strength (50 MPa). The soaking of the cement in a simulated body fluid (SBF) formed a layer of hydroxyapatite like crystals in the surface of the samples. (author)

  7. Defluoridation of drinking water by boiling with brushite and calcite.

    Science.gov (United States)

    Larsen, M J; Pearce, E I F

    2002-01-01

    Existing methods for defluoridating drinking water involve expensive high technology or are slow, inefficient and/or unhygienic. A new method is now suggested, encompassing brushite and calcite suspension followed by boiling. Our aim was to examine the efficiency of the method and the chemical reactions involved. Brushite, 0.3-0.5 g, and an equal weight of calcite were suspended in 1 litre water containing 5-20 ppm fluoride. The suspensions were boiled in an electric kettle, left to cool and the calcium salts to sediment. Solution ion concentrations were determined and sediments were examined by X-ray diffraction. In distilled water initially containing 5, 10 and 20 ppm fluoride the concentration was reduced to 0.06, 0.4 and 5.9 ppm, respectively. Using Aarhus tap water which contained 2.6 mmol/l calcium the final concentrations were 1.2, 2.5 and 7.7 ppm, respectively, and runs without calcite gave results similar to those with calcite. Without boiling the fluoride concentration remained unaltered, as did the brushite and calcite salts, despite occasional agitation by hand. All solutions were supersaturated with respect to fluorapatite and hydroxyapatite and close to saturation with respect to brushite. Boiling produced well-crystallised apatite and traces of calcite, while boiling of brushite alone left a poorly crystallised apatite. We conclude that boiling a brushite/calcite suspension rapidly converts the two salts to apatite which incorporates fluoride if present in solution, and that this process may be exploited to defluoridate drinking water.

  8. Deposition of calcium phosphate coatings using condensed phosphates (P2O7(4-) and P3O10(5-)) as phosphate source through induction heating.

    Science.gov (United States)

    Zhou, Huan; Hou, Saisai; Zhang, Mingjie; Yang, Mengmeng; Deng, Linhong; Xiong, Xinbo; Ni, Xinye

    2016-12-01

    In present work condensed phosphates (P2O7(4-) and P3O10(5-)) were used as phosphate source in induction heating to deposit calcium phosphate coatings. The phase, morphology, and composition of different phosphate-related coatings were characterized and compared using XRD, FTIR, and SEM analyses. Results showed that P2O7(4-)formed calcium pyrophosphate hydrate coatings with interconnected cuboid-like particles. The as-deposited calcium tripolyphosphate hydrate coating with P3O10(5-) was mainly composed of flower-like particles assembled by plate-like crystals. The bioactivity and cytocompatibility of the coatings were also studied. Moreover, the feasibility of using hybrid phosphate sources for preparing and depositing coatings onto magnesium alloy was investigated.

  9. Penggunaan batuan fosfat NDCP (natural defluorinated calcium phosphate sebagai pengganti dicalcium phosphate dalam ransom ayam broiler

    Directory of Open Access Journals (Sweden)

    Arnold P. Sinurat

    1995-08-01

    Full Text Available An experiment was conducted to study the utilization of local rock phosphate or natural defluorinated calcium phosphate (NDCP as phosphorus source for broilers by using the imported dicalcium phosphate (DCP as a reference. The study was designed by formulating 6 experimental diets which consist of 2 phosphorus sources (DCP dan NDCP and 3 dietary total P levels (0 .55 ; 0.65 and 0 .75%. Each diet was fed to 60 chickens (10 replicates with 6 birds each from three day old to 6 weeks of age. Parameters observed were feed consumption, body weight gain, mortality, Ca and P retention, and ash content of tibia bones. Results showed that dietary phosphorus levels (0.55 to 0.75% did not significantly affect body weight gain, feed consumption, and mortalities. However, better feed conversion ratio was obtained when dietary phosphorus level was 0.55%. The NDCP treated birds could significantly gain heavier weight compared with those received DCP, although this improvement was also followed by an increase in the feed consumption. The relative biological value of phosphorus in NDCP was 101 `7n. It is concluded that NDCP can he used in broilers diet to replace DCP as phosphorus source.

  10. Osteoregenerative capacities of dicalcium phosphate-rich calcium phosphate bone cement.

    Science.gov (United States)

    Ko, Chia-Ling; Chen, Jian-Chih; Tien, Yin-Chun; Hung, Chun-Cheng; Wang, Jen-Chyan; Chen, Wen-Cheng

    2015-01-01

    Calcium phosphate cement (CPC) is a widely used bone substitute. However, CPC application is limited by poor bioresorption, which is attributed to apatite, the stable product. This study aims to systematically survey the biological performance of dicalcium phosphate (DCP)-rich CPC. DCP-rich CPC exhibited a twofold, surface-modified DCP anhydrous (DCPA)-to-tetracalcium phosphate (TTCP) molar ratio, whereas conventional CPC (c-CPC) showed a onefold, surface unmodified DCPA-to-TTCP molar ratio. Cell adhesion, morphology, viability, and alkaline phosphatase (ALP) activity in the two CPCs were examined with bone cell progenitor D1 cultured in vitro. Microcomputed tomography and histological observation were conducted after CPC implantation in vivo to analyze the residual implant ratio and new bone formation rate. D1 cells cultured on DCP-rich CPC surfaces exhibited higher cell viability, ALP activity, and ALP quantity than c-CPC. Histological evaluation indicated that DCP-rich CPC showed lesser residual implant and higher new bone formation rate than c-CPC. Therefore, DCP-rich CPC can improve bioresorption. The newly developed DCP-rich CPC exhibited potential therapeutic applications for bone reconstruction.

  11. Randomized crossover study comparing the phosphate-binding efficacy of calcium ketoglutarate versus calcium carbonate in patients on chronic hemodialysis

    DEFF Research Database (Denmark)

    Bro, S; Rasmussen, R A; Handberg, J

    1998-01-01

    The objective of the study was to evaluate the phosphate-binding efficacy, side effects, and cost of therapy of calcium ketoglutarate granulate as compared with calcium carbonate tablets in patients on chronic hemodialysis. The study design used was a randomized, crossover open trial, and the main...

  12. The utilization of rock phosphate (natural defluorinated calcium phosphate or NDCP in laying hens diet to replace dicalcium phosphate

    Directory of Open Access Journals (Sweden)

    A.P Sinurat

    1996-06-01

    Full Text Available An experimentwas conducted to study the utilization of local rock phosphate or natural defluorinated calcium phosphate (NDCP as phosphorus source for layer chickens by using the imported dicalcium phosphate (DCP as a reference. Eight experimental diets consisted of 2 source of phosphorus (DCP and NDCP and 4 dietary total P levels (0.4, 0.5, 0.6 and 0.7% were formulated. Each diet was fed to 24 pullets (6 replicates with 4 birds each from 20 weeks of age to 14 weeks of egg production. Observations were made on feed consumption, egg production, egg weight, mortality, egg quality, Ca and P retention and ash content of tibial bones . Results showed no significant effect of different source and level of phosphorus tested on egg production (% HD, feed consumption, egg weight and mortality rates . Egg shell thickness was depressed in NDCP diet as compared with DCP, however this only occurred at firstmonth of production. It is concluded that the NDCP can be used in layers diet to replace DCP as phosphorus source. The relative biological value of phosphorus inNDCP is 96% for layers.

  13. Polymeric additives to enhance the functional properties of calcium phosphate cements

    Directory of Open Access Journals (Sweden)

    Roman A Perez

    2012-12-01

    Full Text Available The vast majority of materials used in bone tissue engineering and regenerative medicine are based on calcium phosphates due to their similarity with the mineral phase of natural bone. Among them, calcium phosphate cements, which are composed of a powder and a liquid that are mixed to obtain a moldable paste, are widely used. These calcium phosphate cement pastes can be injected using minimally invasive surgery and adapt to the shape of the defect, resulting in an entangled network of calcium phosphate crystals. Adding an organic phase to the calcium phosphate cement formulation is a very powerful strategy to enhance some of the properties of these materials. Adding some water-soluble biocompatible polymers in the calcium phosphate cement liquid or powder phase improves physicochemical and mechanical properties, such as injectability, cohesion, and toughness. Moreover, adding specific polymers can enhance the biological response and the resorption rate of the material. The goal of this study is to overview the most relevant advances in this field, focusing on the different types of polymers that have been used to enhance specific calcium phosphate cement properties.

  14. Effects of fibre reinforcement on the mechanical properties of brushite cement.

    Science.gov (United States)

    Gorst, N J S; Perrie, Y; Gbureck, U; Hutton, A L; Hofmann, M P; Grover, L M; Barralet, J E

    2006-01-01

    In this study the effect of structure and amount of polyglactin fibre incorporation into a brushite forming calcium phosphate cement system and the effect of mechanical compaction on the fibre modified system were investigated. In comparison the effect of resorbable polycaprolactone surface coating of cement specimens was investigated. The results showed that, apart from the mechanical properties of the reinforcing material, the structure of the incorporated fibres, regular or random, is crucial for the resulting flexural strength and modulus of elasticity. Fibre reinforcement could also be combined with mechanical compaction of the cement/fibre composite paste leading to a possible 7-fold increase in flexural strength or an almost 5-fold increase in modulus of elasticity. Reinforcement of the tensile surface of cement grafts may ultimately improve strength where required, especially in conjunction with bone fixation devices.

  15. Structure, properties and animal study of a calcium phosphate/calcium sulfate composite cement.

    Science.gov (United States)

    Chen, Wei-Luen; Chen, Chang-Keng; Lee, Jing-Wei; Lee, Yu-Ling; Ju, Chien-Ping; Lin, Jiin-Huey Chern

    2014-04-01

    In-vitro and in-vivo studies have been conducted on an in-house-developed tetracalcium phosphate (TTCP)/dicalcium phosphate anhydrous (DCPA)/calcium sulfate hemihydrate (CSH)-derived composite cement. Unlike most commercial calcium-based cement pastes, the investigated cement paste can be directly injected into water and harden without dispersion. The viability value of cells incubated with a conditioned medium of cement extraction is >90% that of Al2O3 control and >80% that of blank medium. Histological examination reveals excellent bonding between host bone and cement without interposition of fibrous tissues. At 12 weeks-post implantation, significant remodeling activities are found and a new bone network is developed within the femoral defect. The 26-week samples show that the newly formed bone becomes more mature, while the interface between residual cement and the new bone appears less identifiable. Image analysis indicates that the resorption rate of the present cement is much higher than that of TTCP or TTCP/DCPA-derived cement under similar implantation conditions.

  16. Mechanical and In Vitro Biocompatibility of Brushite Cement Modified by Polyethylene Glycol.

    Science.gov (United States)

    Roy, Mangal; Devoe, Ken; Bandyopadhyay, Amit; Bose, Susmita

    2012-12-01

    Brushite (dicalcium phosphate dihydrate, DCPD) cement, owing to its high solubility in physiological condition and ability to guide new bone formation, is widely used to treat bone defects. In the present study, we have evaluated the effects of poly ethylene glycol (PEG) addition on the setting time, compressive strength and in vitro biocompatibility of brushite cement. The brushite cements were prepared by mixing β-tricalcium phosphate [β-TCP, Ca(3)(PO(4))(2)] and monocalcium phosphate monohydrate [MCPM, Ca(H(2)PO(4))(2). H(2)O]. PEG was introduced at 2.0 and 5.0 wt% with the liquid. Introduction of PEG resulted in marginal increase in both initial and final setting time; however, significantly affected the compressive strength. Effects of PEG incorporation on in vitro biocompatibility of brushite cements were studied by using human fetal osteoblast cells (hFOB) cells. Field emission scanning electron microscope (FESEM) images and immunohistochemical analysis indicated that pure and PEG incorporated brushite cement facilitates cell adhesion, proliferation and differentiation. Fewer cells expressed vinculin protein with increased PEG content in the cement. Cell proliferation was found to decrease with increased PEG concentration while the cell differentiation increased with PEG content. Our results provide a better understanding of in vitro biocompatibility of PEG added brushite cements that can be used to customize the cement compositions based on application need.

  17. Novel rechargeable calcium phosphate nanoparticle-containing orthodontic cement.

    Science.gov (United States)

    Xie, Xian-Ju; Xing, Dan; Wang, Lin; Zhou, Han; Weir, Michael D; Bai, Yu-Xing; Xu, Hockin Hk

    2016-11-04

    White spot lesions (WSLs), due to enamel demineralization, occur frequently in orthodontic treatment. We recently developed a novel rechargeable dental composite containing nanoparticles of amorphous calcium phosphate (NACP) with long-term calcium (Ca) and phosphate (P) ion release and caries-inhibiting capability. The objectives of this study were to develop the first NACP-rechargeable orthodontic cement and investigate the effects of recharge duration and frequency on the efficacy of ion re-release. The rechargeable cement consisted of pyromellitic glycerol dimethacrylate (PMGDM) and ethoxylated bisphenol A dimethacrylate (EBPADMA). NACP was mixed into the resin at 40% by mass. Specimens were tested for orthodontic bracket shear bond strength (SBS) to enamel, Ca and P ion initial release, recharge and re-release. The new orthodontic cement exhibited an SBS similar to commercial orthodontic cement without CaP release (P>0.1). Specimens after one recharge treatment (e.g., 1 min immersion in recharge solution repeating three times in one day, referred to as "1 min 3 times") exhibited a substantial and continuous re-release of Ca and P ions for 14 days without further recharge. The ion re-release did not decrease with increasing the number of recharge/re-release cycles (P>0.1). The ion re-release concentrations at 14 days versus various recharge treatments were as follows: 1 min 3 times>3 min 2 times>1 min 2 times>6 min 1 time>3 min 1 time>1 min 1 time. In conclusion, although previous studies have shown that NACP nanocomposite remineralized tooth lesions and inhibited caries, the present study developed the first orthodontic cement with Ca and P ion recharge and long-term release capability. This NACP-rechargeable orthodontic cement is a promising therapy to inhibit enamel demineralization and WSLs around orthodontic brackets.International Journal of Oral Science advance online publication,4 November 2016; doi:10.1038/ijos.2016.40.

  18. Mechanical and fracture behavior of calcium phosphate cements

    Science.gov (United States)

    Jew, Victoria Chou

    Apatite-based calcium phosphate cements are currently employed to a limited extent in the biomedical and dental fields. They present significant potential for a much broader range of applications, particularly as a bone mineral substitute for fracture fixation. Specifically, hydroxyapatite (HA) is known for its biocompatibility and non-immunogenicity, attributed to its similarity to the mineral phase of natural bone. The advantages of a cement-based HA include injectability, greater resorbability and osteoconductivity compared to sintered HA, and an isothermal cement-forming reaction that avoids necrosis during cement setting. Although apatite cements demonstrate good compressive strength, tensile properties are very weak compared to natural bone. Applications involving normal weight-bearing require better structural integrity than apatite cements currently provide. A more thorough understanding of fracture behavior can elucidate failure mechanisms and is essential for the design of targeted strengthening methods. This study investigated a hydroxyapatite cement using a fracture mechanics approach, focusing on subcritical crack growth properties. Subcritical crack growth can lead to much lower load-bearing ability than critical strength values predict. Experiments show that HA cement is susceptible to crack growth under both cyclic fatigue-crack growth and stress corrosion cracking conditions, but only environmental, not mechanical, mechanisms contribute to crack extension. This appears to be the first evidence ever presented of stress corrosion crack growth behavior in calcium phosphate cements. Stress corrosion cracking was examined for a range of environmental conditions. Variations in pH have surprisingly little effect. Behavior in water at elevated temperature (50°C) is altered compared to water at ambient temperature (22°C), but only for crack-growth velocities below 10-7 m/s. However, fracture resistance of dried HA cement in air increases significantly

  19. Preparation of in situ hardening composite microcarriers: calcium phosphate cement combined with alginate for bone regeneration.

    Science.gov (United States)

    Park, Jung-Hui; Lee, Eun-Jung; Knowles, Jonathan C; Kim, Hae-Won

    2014-03-01

    Novel microcarriers consisting of calcium phosphate cement and alginate were prepared for use as three-dimensional scaffolds for the culture and expansion of cells that are effective for bone tissue engineering. The calcium phosphate cement-alginate composite microcarriers were produced by an emulsification of the composite aqueous solutions mixed at varying ratios (calcium phosphate cement powder/alginate solution = 0.8-1.2) in an oil bath and the subsequent in situ hardening of the compositions during spherodization. Moreover, a porous structure could be easily created in the solid microcarriers by soaking the produced microcarriers in water and a subsequent freeze-drying process. Bone mineral-like apatite nanocrystallites were shown to rapidly develop on the calcium phosphate cement-alginate microcarriers under moist conditions due to the conversion of the α-tricalcium phosphate phase in the calcium phosphate cement into a carbonate-hydroxyapatite. Osteoblastic cells cultured on the microspherical scaffolds were proven to be viable, with an active proliferative potential during 14 days of culture, and their osteogenic differentiation was confirmed by the determination of alkaline phosphatase activity. The in situ hardening calcium phosphate cement-alginate microcarriers developed herein may be used as potential three-dimensional scaffolds for cell delivery and tissue engineering of bone.

  20. Degree of vinyl conversion in experimental amorphous calcium phosphate composites

    Science.gov (United States)

    Tarle, Z.; Knežević, A.; Matošević, D.; Škrtić, D.; Ristić, M.; Prskalo, K.; Musić, S.

    2009-04-01

    An experimental dental composite, based on amorphous calcium phosphate (ACP) with the potential to arrest caries development and regenerate mineral-deficient tooth structures has recently been developed. The aim of this study was to assess the degree of vinyl conversion (DVC) attained in experimental composites based on zirconia-modified ACP. Photo-activated resins were based on ethoxylated bisphenol A dimethacrylate (EBPADMA) [ETHM series with varying EBPADMA/triethylene glycol dimethacrylate (TEGDMA) molar ratios assigned 0.5-ETHM I, 0.85-ETHM II and 1.35-ETHM III], or 2,2-bis[p-(2'-hydroxy-3'-methacryloxypropoxy)phenyl]-propane (Bis-GMA) [BTHZ series]. To asses a possible effect of filler particle size on DVC, composites containing 60 mass % resin and 40 mass % of either milled ACP (mACP; median diameter d m = 0.9 μm) or coarse ACP (cACP; d m = 6.0 μm) were prepared, and irradiated with LED curing unit for 40 s. The DVC was calculated as the % change in the ratio of the integrated peak areas between the aliphatic and aromatic absorption bands determined by Fourier transform infrared spectroscopy (FTIR). The highest DVCs values were attained in mACP-BTHZ, cACP-BTHZ and mACP-ETHM III formulations. DVC of tested ACP composites (on average (76.76 ± 4.43)%) compares well with or exceeds DVCs values reported for the majority of commercial materials.

  1. Structure and properties of silver-doped calcium phosphate nanopowders

    Indian Academy of Sciences (India)

    RAVINDER PAL SINGH; UMA BATRA

    2016-09-01

    Stable and antimicrobial silver-doped calcium phosphate nanopowders were synthesized using sol–gel route by setting the atomic ratio of Ag/(Ag +Ca) at 3%and (Ca $+$ Ag)/P at 1.67. Prior to synthesis of nanopowders, influence of time of hydrolyzation on pH and density of precursors were comprehensively studied. Hydrolyzation time was found to have profound influence on pH of constituent precursors. Sufficient hydrolysis resulted in early maturation of sol. Scanning electron microscopy (SEM) showed the heterogeneous and agglomerated state of particles with average size of $3.9\\pm 1.9$ $\\mu$m. Energy dispersive X-ray spectroscopy (EDX) presented uniform distributionof O, Ag, Ca and P elements in nanopowder. Fourier transform infrared spectroscopy (FTIR) confirmed the formation of apatitic structure, whereas X-ray diffraction (XRD) revealed the multiphase constitution of nanopowdersprimarily composed of $\\beta$-TCP, Ag and other hybrid phases. Crystallite size and lattice parameters of $\\beta$-TCP and Ag phases were increased with the rise in calcination temperature. Thermogravimetric analysis (TGA) showed threeregions of weight change and indicated the high thermal stability of nanopowders. Disk diffusion method was used to test the antimicrobial resistance of nanopowders against Escherichia coli and Staphylococcus aureus bacterial strains. All nanopowders exhibited antimicrobial resistance against both E. coli and S. aureus bacteria.

  2. Initial Stability Study of Calcium Phosphate Coated Dental Implants

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Thin film of biodegradable calcium phosphate coated on threaded commercially pure titanium( cp- Ti) dental implants has been investigated as one of alternatives to eliminate the problem of the long-term instability of plasma sprayed HA coated implants. In order to compare in-vivo hone-to-implant response behavior among as-machined, HA coated and CMP coated groups, each group was implanted into New Zealand white mature male rabbits for 2 and 6 weeks, and then in- vivo biological behavior was examined in terms of H&E staining. Initial stability and removable torques of implants were compared among three groups. Measured removable torque of CMP coated specimen at 6 wceks after implantation was significantly higher than that of non-coated group, but slightly lower than that of HA coated group, without any inflammatory response at the surrounding of the implants. The initial stability (ISQ value; implant stability quotient ) of CMP coated specimen at 2 weeks after implantation was slightly lower than that of HA coated group and significantly higher than that of non-coated group. However, after 6 weeks, ISQ value of CMP coated group was slightly higher than that of HA coated group and significantly higher than that of non-coated group.

  3. Calcium phosphates in biomedical applications: materials for the future?

    Directory of Open Access Journals (Sweden)

    Wouter Habraken

    2016-03-01

    Full Text Available Our populations are aging. Some experts predict that 30% of hospital beds will soon be occupied by osteoporosis patients. Statistics show that 20% of patients suffering from an osteoporotic hip fracture do not survive the first year after surgery, all this showing that there is a tremendous need for better therapies for diseased and damaged bone. Human bone consists for about 70% of calcium phosphate (CaP mineral, therefore CaPs are the materials of choice to repair damaged bone. To do this successfully, the process of CaP biomineralization and the interaction of CaPs and biological environment in the body need to be fully understood. First commercial CaP bone graft substitutes were launched 40 years ago, and they are currently often regarded as ‘old biomaterials’ or even as an ‘obsolete’ research topic. Some even talk about ‘stones’. The aim of this manuscript is to highlight the tremendous improvements achieved in CaP materials research in the past 15 years, in particular in the field of biomineralization, as carrier for gene or ion delivery, as biologically active agent, and as bone graft substitute. Besides an outstanding biological performance, CaPs are easily and inexpensively produced, are safe, and can be relatively easily certified for clinical use. As such, CaP materials have won their spurs, but they also offer a great promise for the future.

  4. Randomized crossover study comparing the phosphate-binding efficacy of calcium ketoglutarate versus calcium carbonate in patients on chronic hemodialysis.

    Science.gov (United States)

    Bro, S; Rasmussen, R A; Handberg, J; Olgaard, K; Feldt-Rasmussen, B

    1998-02-01

    The objective of the study was to evaluate the phosphate-binding efficacy, side effects, and cost of therapy of calcium ketoglutarate granulate as compared with calcium carbonate tablets in patients on chronic hemodialysis. The study design used was a randomized, crossover open trial, and the main outcome measurements were plasma ionized calcium levels, plasma phosphate levels, plasma intact parathyroid hormone (PTH) levels, requirements for supplemental aluminum-aminoacetate therapy, patient tolerance, and cost of therapy. Nineteen patients on chronic hemodialysis were treated with a dialysate calcium concentration of 1.25 mmol/L and a fixed alfacalcidol dose for at least 2 months. All had previously tolerated therapy with calcium carbonate. Of the 19 patients included, 10 completed both treatment arms. After 12 weeks of therapy, the mean (+/-SEM) plasma ionized calcium level was significantly lower in the ketoglutarate arm compared with the calcium carbonate arm (4.8+/-0.1 mg/dL v 5.2+/-0.1 mg/dL; P = 0.004), whereas the mean plasma phosphate (4.5+/-0.3 mg/dL v 5.1+/-0.1 mg/dL) and PTH levels (266+/-125 pg/mL v 301+/-148 pg/mL) did not differ significantly between the two treatment arms. Supplemental aluminum-aminoacetate was not required during calcium ketoglutarate treatment, while two patients needed this supplement when treated with calcium carbonate. Five of 17 (29%) patients were withdrawn from calcium ketoglutarate therapy within 1 to 2 weeks due to intolerance (anorexia, vomiting, diarrhea, general uneasiness), whereas the remaining 12 patients did not experience any side effects at all. The five patients with calcium ketoglutarate intolerance all had pre-existing gastrointestinal symptoms; four of them had received treatment with cimetidine or omeprazol before inclusion into the study. Calculations based on median doses after 12 weeks showed that the cost of the therapy in Denmark was 10 times higher for calcium ketoglutarate compared with calcium

  5. Evaluation of Calcium Phosphate Cement As a Root Canal Sealer Filling Material

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Calcium phosphate cement for root end sealing was obtained by mixing α-tricalcium phosphate and additives with an aqueous solution of citric. Powder and liquid were mixed at a ratio of 1.25g/mL. The biocompatibility of this material was investigated primarily by subcutaneous implantation tests. Then calcium phosphate cement was used to fill three adult dogs' root canal, both calcium hydroxide paste and hydroxyapatite paste as control. The animals were killed at 4,12,20 weeks postoperatively respectively. The effects of different materials on the apical closure, restoration of periapical tissues and adaptability to the dentinal surface were examined by optical and electronic microscope. The observation at 20 weeks shows that the calcium phosphate cement has the potentialities of being a root canal sealer filling material available for pulpless teeth with open-apex and destructive periapical tissue.

  6. Reflections on the Mechanism of Calcium Phosphate Nucleation on Titanium in Simulated Body Fluids

    Institute of Scientific and Technical Information of China (English)

    F. T. Cheng

    2005-01-01

    The results and main findings of studies reported in the literature in relation to the deposition of calcium phosphate on Ti in simulated body fluids are summarized. The effects of the surface hydroxyl groups and the sign of surface charge on the nucleation of calcium phosphate are reviewed. One major controversy among the conclusions of different studies is the order of adsorption of the calcium ions and the phosphate ions in the initial stage of immersion. A simple model based on the amphoteric nature of the hydroxyl groups on Ti is proposed in an attempt to delineate the nucleation process for calcium phosphate on Ti in simulated body fluids. HPO42- ions interact with the hydroxyl groups via ion exchange and/or electrostatic attraction, and Ca2+ ions, via electrostatic attraction only. There is no preferential order of adsorption. Seemingly inconsistent results in different studies possibly arise from different prior treatments of the samples, which affect the adsorption properties.

  7. Gelation and biocompatibility of injectable alginate-calcium phosphate gels for bone regeneration

    NARCIS (Netherlands)

    Cardoso, D.A.; Beucken, J.J.J.P van den; Both, L.L.; Bender, J.; Jansen, J.A.; Leeuwenburgh, S.C.G.

    2014-01-01

    An emerging approach toward development of injectable, self-setting, and fully biodegradable bone substitutes involves the combination of injectable hydrogel matrices with a dispersed phase consisting of nanosized calcium phosphate particles. Here, novel injectable composites for bone regeneration h

  8. Balloon vetebroplasty with calcium phosphate cement augmentation for direct restoration of traumatic thoracolumbar vertebral fractures

    NARCIS (Netherlands)

    Verlaan, JJ; van Helden, WH; Oner, FC; Verbout, AJ; Dhert, WJA

    2002-01-01

    Study Design. A human cadaveric model was used to evaluate balloon vertebroplasty in traumatic vertebral fractures. Objectives. To assess the feasibility and safety of balloon vertebroplasty followed by calcium phosphate cement augmentation to prevent recurrent kyphosis. Summary of Background Data.

  9. Towards understanding biomineralization:calcium phosphate in a biomimetic minerallzation process

    Institute of Scientific and Technical Information of China (English)

    Yu-rong CAI; Rui-kang TANG

    2009-01-01

    Biomineralization processes result in organic/inorganic hybrid materials with complex shapes,hiemrchi-cal structures.and superior matefial properties. Recent developments in biominemlization and biomatarials have demonstrated that calcium phosphate particles play an important role in the formation of hard tissues in nature. In this paper,current concepts in biominemlization,such as nano assembly,biomimetic shell structure,and their applications are introduced. It is confirmed experimentally that enamel-or bone-liked apatita can be achieved by oriented aggregations using nano calcium phosphates as starting matarials. The assembly of calcium phosphate can be either promoted or inhibited by diflerent biomolecules so that the kinetics can he regulated biologically.In this paper,the role of nano calcium phosphate in tissue repair is highligllted Furthermore,a new,interesting result on biomimetie mineralization 1s Introduced,which can offer an artificial shell for living cells via a biomimatic method .

  10. Characterization of a silver-incorporated calcium phosphate film by RBS and its antimicrobial effects

    Energy Technology Data Exchange (ETDEWEB)

    Han, I-H [Institute of Physics and Applied Physics, and Atomic-Scale Surface Science Research Center, Yonsei University, Seou1 120-749 (Korea, Republic of); Lee, I-S [Institute of Physics and Applied Physics, and Atomic-Scale Surface Science Research Center, Yonsei University, Seou1 120-749 (Korea, Republic of); Song, J-H [Advanced Analysis Center, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Lee, M-H [Department of Medical Engineering, Yonsei University, Seoul 120-752 (Korea, Republic of); Park, J-C [Department of Medical Engineering, Yonsei University, Seoul 120-752 (Korea, Republic of); Lee, G-H [Korea Institute of Machinery and Materials, Chang-Won 641-010 (Korea, Republic of); Sun, X-D [Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Chung, S-M [Implantium Research Center, Seoul 135-879 (Korea, Republic of)

    2007-09-15

    A thin calcium phosphate film was synthesized on both commercially pure Ti and Si wafers by electron beam evaporation of hydroxyapatite as an evaporant with simultaneous Ar ion beam bombardments. Silver was introduced into an ion-beam-assisted deposition of a calcium phosphate thin film for antimicrobial effect. The amount of incorporated silver ions was controlled by immersing calcium-phosphate-coated samples in different AgNO{sub 3} concentrations, and Rutherford backscattering spectrometry (RBS) was employed to measure the amounts of substituted silver. The higher concentration of silver in the calcium phosphate film was more effective in reducing the bacteria of Escherichia coli ATCC 8739 and Streptococcus mutans OMZ 65 on contact with respect to controls.

  11. Relationship between Salivary Alkaline Phosphatase Enzyme Activity and The Concentrations of Salivary Calcium and Phosphate Ions

    Directory of Open Access Journals (Sweden)

    Mina Jazaeri

    2015-04-01

    Full Text Available Although salivary alkaline phosphatase (ALP can balance de- and remineralization processes of enamel, there is no evidence regarding its effects on the concentrations of calcium and phosphate in saliva. The present study aims to determine the relationship between salivary ALP activity and the concentrations of calcium and phosphate in saliva. In this cross-sectional study, we evaluated salivary markers in 120 males, ages 19 to 44 years. All participants provided 5 mL of unstimulated whole saliva and the level of enzyme activity as well as calcium and phosphate concentrations were measured using a colorimetric method. Data were gathered and analyzed by statistical package for social sciences (SPSS 13.00 using Pearson correlation test. A p value of 0.05. According to the results of the present study, there was no significant relation between salivary ALP activity and calcium and phosphate concentrations in saliva. However, further research is highly recommended.

  12. Effect of Reaction Pathway on the Extent and Mechanism of Uranium(VI) Immobilization with Calcium and Phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Mehta, Vrajesh S.; Maillot, Fabien; Wang, Zheming; Catalano, Jeffrey G.; Giammar, Daniel E.

    2016-03-15

    Phosphate addition to subsurface environments contaminated with uranium can be used as an in situ remediation approach. Batch experiments were conducted to evaluate the dependence of the extent and mechanism of uranium uptake on the pathway for reaction with calcium phosphates. At pH 4.0 and 6.0 uranium uptake occurred via autunite (Ca(UO2)(PO4)3) precipitation irrespective of the starting forms of calcium and phosphate. At pH 7.5, the uptake mechanism depended on the nature of the calcium and phosphate. When dissolved uranium, calcium, and phosphate were added simultaneously, uranium was structurally incorporated into a newly formed amorphous calcium phosphate solid. Adsorption was the dominant removal mechanism for uranium contacted with pre-formed amorphous calcium phosphate solids,. When U(VI) was added to a suspension containing amorphous calcium phosphate solids as well as dissolved calcium and phosphate, then removal occurred through precipitation (57±4 %) of autunite and adsorption (43±4 %) onto calcium phosphate. The solid phase speciation of the uranium was determined using X-ray absorption spectroscopy and laser induced fluorescence spectroscopy. Dissolved uranium, calcium, and phosphate concentrations with saturation index calculations helped identify removal mechanisms and determine thermodynamically favorable solid phases.

  13. Physicochemical and Microstructural Characterization of Injectable Load-Bearing Calcium Phosphate Scaffold

    OpenAIRE

    Mazen Alshaaer; Kailani, Mohammed H.; Hanan Jafar; Nidaa Ababneh; Abdalla Awidi

    2013-01-01

    Injectable load-bearing calcium phosphate scaffolds are synthesized using rod-like mannitol grains as porogen. These degradable injectable strong porous scaffolds, prepared by calcium phosphate cement, could represent a valid solution to achieve adequate porosity requirements while providing adequate support in load-bearing applications. The proposed process for preparing porous injectable scaffolds is as quick and versatile as conventional technologies. Using this method, porous CDHA-based c...

  14. Calcium phosphate formation from sea urchin - (brissus latecarinatus) via modified mechano-chemical (ultrasonic) conversion method

    OpenAIRE

    R. Samur; Ozyegin, L.; D. Agaogullari; F. N. Oktar; Agathopoulos, S.; Kalkandelen, C.; I. Duman; B. Ben-Nissan

    2013-01-01

    This study aims to produce apatite structures, such as hydroxyapatite (HA) and fluorapatite (FA), from precursor calcium phosphates of biological origin, namely from sea urchin, with mechano-chemical stirring and hot-plating conversion method. The produced materials were heat treated at 800 °C for 4 hours. X-ray diffraction and scanning electron microscopy (SEM) studies were conducted. Calcium phosphate phases were developed. The SEM images showed the formation of micro to nano-powders. The e...

  15. Preparation and characterization of a novel injectable strontium-containing calcium phosphate cement with collagen

    OpenAIRE

    2015-01-01

    Purpose: To develop a novel injectable strontium-containing calcium phosphate cement with collagen. Methods: A novel calcium phosphate bone cement (CPC) was prepared with the addition of strontium element, collagenⅠ, and modified starch; the injectability, solidification time, microstructure, phase composition, compressive strength, anti-collapsibility and histological properties of material were evaluated. Results: The results showed that the material could be injected with an excellen...

  16. Influence of Ethylene Glycol on the Formation of Calcium Phosphate Nanocrystals

    Institute of Scientific and Technical Information of China (English)

    Yi ZUO; Yubao LI; Jie WEI; Yonggang YAN

    2003-01-01

    A synthesis route of using calcium hydroxide Ca(OH)2 with ethylene glycol solvent and orthophosphoric acid (H3PO4)as reagents is described. Three ratios of ethylene glycol to distilled water 1:0, 1:1 and 0:1 are used as diluting media for Ca(OH)2. Crystals of different morphology and composition are formed under weak alkaline circumstance at pH 7.0~8.0. Acicular calcium phosphate nanocrystals are prepared in pure ethylene glycol while rod-like calcium phosphate nanocrystals form in pure distilled water. The nanograde size of the former is smaller than that of the latter. Calcium-deficient apatite (CDAP) is obtained with a Ca/P molar ratio of 1.66. Therefore, it was deduced that the usage of ethylene glycol solvent could influence the formation of calcium phosphate crystal lattice.

  17. Simplified estimates of ion-activity products of calcium oxalate and calcium phosphate in mouse urine.

    Science.gov (United States)

    Tiselius, Hans-Göran; Ferraz, Renato Ribeiro Nogueira; Heilberg, Ita Pfeferman

    2012-08-01

    This study aimed at formulating simplified estimates of ion-activity products of calcium oxalate (AP(CaOx)) and calcium phosphate (AP(CaP)) in mouse urineto find the most important determinants in order to limit the analytical work-up. Literature data on mouse urine composition was used to determine the relative effect of each urine variable on the two ion-activity products. AP(CaOx) and AP(CaP) were calculated by iterative approximation with the EQUIL2 computerized program. The most important determinants for AP(CaOx) were calcium, oxalate and citrate and for AP(CaP) calcium, phosphate, citrate, magnesium and pH. Urine concentrations of the variables were used. A simplified estimate of AP(CaOx) (AP(CaOx)-index(MOUSE)) that numerically approximately corresponded to 10(8) × AP(CaOx) was given the following expression:[Formula: see text]For a series of urine samples with various composition the coefficient of correlation between AP(CaOx)-index(MOUSE) and 10(8) × AP(CaOx) was 0.99 (p = 0.00000). A similar estimate of AP(CaP) (AP(CaP)-index(MOUSE)) was formulated so that it approximately would correspond numerically to 10(14) × AP(CaP) taking the following form:[Formula: see text]For a series of variations in urine composition the coefficient of correlation was 0.95 (p = 0.00000). The two approximate estimates shown in this article are simplified expressions of AP(CaOx) and AP(CaP). The intention of these theoretical calculations was not to get methods for accurate information on the saturation levels in urine, but to have mathematical tools useful for rough conclusions on the outcome of different experimental situations in mice. It needs to be emphasized that the accuracy will be negatively influenced if urine variables not included in the formulas differ very much from basic concentrations.

  18. Characterization of alginate-brushite in-situ hydrogel composites.

    Science.gov (United States)

    Dabiri, Seyed Mohammad Hossein; Lagazzo, Alberto; Barberis, Fabrizio; Farokhi, Mehdi; Finochio, Elisabetta; Pastorino, Laura

    2016-10-01

    In the present study alginate-brushite composite hydrogels were in-situ synthetized and characterized with respect to preparation parameters. Specifically, the influence of initial pH value and initial concentration of phosphate precursor on the in-situ fabrication of the composite hydrogel were taken into account. The composite hydrogels were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric (TGA, DTG) and differential thermal analysis (DTA). Finally, the cell viability tests were carried out (MTT) over the incubation time period of 3, 7, and 14days. The results revealed that the formation and the crystalline stability of brushite were highly dependent on the initial pH value. It was shown that as the pH reached to the value of 6, characteristics peaks of brushite appeared in the FTIR spectra. Besides, the XRD and thermal analysis results were in a good accordance with those of FTIR. In addition, the SEM images demonstrated that the plate like brushite was formed inside the alginate matrix. Also, a considerable impact of pH variation on the biocompatibility of samples was noticed so that the majority of samples especially those prepared in the acidic conditions were toxic.

  19. An Understanding of Renal Stone Development in a Mixed Oxalate–Phosphate System

    Science.gov (United States)

    Guan, Xiangying; Wang, Lijun; Dosen, Anja; Tang, Ruikang; Giese, Rossman F.; Giocondi, Jennifer L.; Orme, Christine A.; Hoyer, John R.; Nancollas, George H.

    2009-01-01

    The in vivo formation of calcium oxalate concretions having calcium phosphate nidi is simulated in an in vitro (37 °C, pH 6.0) dual constant composition (DCC) system undersaturated (σDCPD = −0.330) with respect to brushite (DCPD, CaHPO4 · 2H2O) and slightly supersaturated (σCOM = 0.328) with respect to calcium oxalate monohydrate (COM, CaC2O4 · H2O). The brushite dissolution provides calcium ions that raise the COM supersaturation, which is heterogeneously nucleated either on or near the surface of the dissolving calcium phosphate crystals. The COM crystallites may then aggregate, simulating kidney stone formation. Interestingly, two intermediate phases, anhydrous dicalcium phosphate (monetite, CaHPO4) and calcium oxalate trihydrate (COT), are also detected by X-ray diffraction during this brushite–COM transformation. In support of clinical observations, the results of these studies demonstrate the participation of calcium phosphate phases in COM crystallization providing a possible physical chemical mechanism for kidney stone formation. PMID:18557638

  20. Study on the bonding strength between calcium phosphate/chitosan composite coatings and a Mg alloy substrate

    Science.gov (United States)

    Zhang, Jie; Dai, Chang-Song; Wei, Jie; Wen, Zhao-Hui

    2012-11-01

    In order to improve the bonding strength between calcium phosphate/chitosan composite coatings and a micro-arc oxidized (MAO)-AZ91D Mg alloy, different influencing parameters were investigated in the process of electrophoretic deposition (EPD) followed by conversion in a phosphate buffer solution (PBS). Surface morphology and phase constituents of the as-prepared materials were investigated by using X-ray diffractometer (XRD), Fourier-transformed infrared spectrophotometer (FTIR), Raman spectrometer, scanning electron microscope (SEM) with an energy dispersive spectrometer (EDS), and a thermo gravimetric and differential thermal analyzer (TG-DTA). Scratch tests were carried out to study the bonding properties between the coatings and the substrates. In vitro immersion tests were conducted to determine the corrosion behaviors of samples with and without deposit layers through electrochemical experiments. In the EPD process, the acetic acid content in the electrophoresis suspension and the electrophoretic voltage played important roles in improving the bonding properties, while the contents of chitosan (CS) and nano-hydroxyapatite (nHA, Ca10(PO4)6(OH)2) in the suspension had less significant influences on the mechanical bonding strength. It was observed that the coatings showed the excellent bonding property when an electrophoretic voltage was in a range of 40-110 V with other reagent amounts as follows: acetic acid: 4.5 vol.%, CS ≤ 0.25 g, nHA ≤ 2.0 g in 200 ml of a CS-acetic acid aqueous solution and nHA ≤ 2.5 g in 300 ml of absolute ethanol. The morphology of the composite coating obtained under the above optimal condition had a flake-like crystal structure. The EPD in the nHA/CS-acetic acid/ethanol suspension resulted in hydroxyapatite, chitosan, brushite (DCPD, CaHPO4·2H2O) and Ca(OH)2 in the coatings. After the as-prepared coating materials were immersed into PBS, Ca(OH)2 could be converted into HA and DCPD. The results of the electrochemical tests

  1. Enzymatic pH control for biomimetic deposition of calcium phosphate coatings

    NARCIS (Netherlands)

    Nijhuis, A.W.G.; Nejadnik, M.R.; Nudelman, F.; Walboomers, X.F.; Riet, J. te; Habibovic, P.; Tahmasebi Birgani, Z.; Li, Y.; Bomans, P.H.; Jansen, J.A.; Sommerdijk, N.A.; Leeuwenburgh, S.C.G.

    2014-01-01

    The current study examines the enzymatic decomposition of urea into carbon dioxide and ammonia as a means to increase the pH during biomimetic deposition of calcium phosphate (CaP) onto implant surfaces. The kinetics of the enzymatically induced pH increase were studied by monitoring pH, calcium con

  2. Low temperature method for the production of calcium phosphate fillers

    Directory of Open Access Journals (Sweden)

    Nastro Alfonso

    2004-03-01

    Full Text Available Abstract Background Calcium phosphate manufactured samples, prepared with hydroxyapatite, are used as either spacers or fillers in orthopedic surgery, but these implants have never been used under conditions of mechanical stress. Similar conditions also apply with cements. Many authors have postulated that cements are a useful substitute material when implanted in vivo. The aim of this research is to develop a low cristalline material similar to bone in porosity and cristallinity. Methods Commercial hydroxyapatite (HAp and monetite (M powders are mixed with water and compacted to produce cylindrical samples. The material is processed at a temperature of 37–120 degrees C in saturated steam to obtain samples that are osteoconductive. The samples are studied by X-ray powder diffraction (XRD, Vickers hardness test (HV, scanning electron microscopy (SEM, and porosity evaluation. Results The X-ray diffractions of powders from the samples show patterns typical of HAp and M powders. After thermal treatment, no new crystal phase is formed and no increase of the relative intensity of the peaks is obtained. Vicker hardness data do not show any relationship with treatment temperature. The total porosity decreases by 50–60% according to the specific thermal treatment. Scanning electron microscopy of the surfaces of the samples with either HAp 80%-M 20% (c or Hap 50%-M 50% (f, show cohesion of the powder grains. Conclusions The dissolution-reprecipitation process is more intesive in manufactured samples (c and (f, according to Vickers hardness data. The process occurs in a steam saturated environment between 37 degrees and 120 degrees C. (c (f manufactured samples show pore dimension distributions useful to cellular repopulation in living tissues.

  3. Zinc phosphate as versatile material for potential biomedical applications Part II.

    Science.gov (United States)

    Herschke, L; Lieberwirth, I; Wegner, G

    2006-01-01

    Surface chemical reactivity of two modifications of synthetic zinc phosphate tetrahydrate (alpha - and beta -form of Hopeite, alpha -,beta -ZPT) has been studied by selective chemical and e-beam etching in presence of diluted phosphoric acid and ammonia by Scanning Electron Microscopy (SEM) and microelectrophoresis (zeta potential measurements) in correlation with the corresponding bulk properties and crystal size distributions. The subtitle crystallographic differences between alpha -and beta -ZPT originating from a unique hydrogen bonding pattern, induce drastic variations of both surface potential and surface charge. Biogenic Hydroxyapatite (HAP) and one of its metastable precursors, a calcium dihydrogen phosphate dihydrate (DCPD) or Brushite were used to underline this resulting variation of chemical reactivity in zinc phosphates. In-situ monitoring of the transformation of Brushite in Hydroxyapatite is also reported.

  4. Calcium carbonate-calcium phosphate mixed cement compositions for bone reconstruction.

    Science.gov (United States)

    Combes, C; Bareille, R; Rey, C

    2006-11-01

    The feasibility of making calcium carbonate-calcium phosphate (CaCO(3)-CaP) mixed cements, comprising at least 40% (w/w) CaCO(3) in the dry powder ingredients, has been demonstrated. Several original cement compositions were obtained by mixing metastable crystalline CaCO(3) phases with metastable amorphous or crystalline CaP powders in aqueous medium. The cements set within at most 1 h at 37 degrees C in atmosphere saturated with water. The hardened cement is microporous and exhibits weak compressive strength. The setting reaction appeared to be essentially related to the formation of a highly carbonated nanocrystalline apatite phase by reaction of the metastable CaP phase with part or almost all of the metastable CaCO(3) phase. The recrystallization of metastable CaP varieties led to a final cement consisting of a highly carbonated poorly crystalline apatite analogous to bone mineral associated with various amounts of vaterite and/or aragonite. The presence of controlled amounts of CaCO(3) with a higher solubility than that of the apatite formed in the well-developed CaP cements might be of interest to increase resorption rates in biomedical cement and favors its replacement by bone tissue. Cytotoxicity testing revealed excellent cytocompatibility of CaCO(3)-CaP mixed cement compositions.

  5. Reactive calcium-phosphate-containing poly(ester-co-ether) methacrylate bone adhesives: setting, degradation and drug release considerations.

    Science.gov (United States)

    Zhao, Xin; Olsen, Irwin; Pratten, Jonathan; Knowles, Jonathan C; Young, Anne M

    2011-09-01

    This study has investigated novel bone adhesives consisting of fluid photo-polymerizable poly(lactide-co-propylene glycol-co-lactide)dimethacrylate (PGLA-DMA) mixed with systematically varying fillers of β-tricalcium phosphate (β-TCP) and monocalcium phosphate monohydrate (MCPM), for the delivery of an antibacterial drug chlorhexidine (CHX). All formulations were found to polymerize fully within 200 s after exposure to blue light. In addition, water sorption by the polymerized materials catalyzed varying filler conversion to dicalcium phosphate (DCP) (i.e. brushite and monetite). With greater DCP levels, faster degradation was observed. Moreover, increase in total filler content enhanced CHX release, associated with higher antibacterial activity. These findings thus suggest that such rapid-setting and degradable adhesives with controllable drug delivery property could have potential clinical value as bone adhesives with antibacterial activity.

  6. Microanalyses of the hydroxyl—poly—calcium sodium phosphate coatings produced by ion beam assisted deposition

    Institute of Scientific and Technical Information of China (English)

    LIUZhong-Yang; WANGChang-Xing; 等

    2002-01-01

    Thin calcium phosphate catings on titanium alloy substrates were prepared by Ar+ ion beam assisted deposition(IBAD) from hydroxyl-poly-calcium sodium phosphate(HPPA) target.The coatings were analyzed by XRD,FTIR,XPS,These analyses revealed that the as-deposited films were amorphous or no apparent crystallinity.No distinct absorption band of the hydroxyl group was observed in FTIR spectra of the coatings but new absorption bands were presented for CO3-2,The calcium to phosphorous ratio of these catings in different IBAD conditions varied from 0.46 to 3.36.

  7. Discrimination between biologically relevant calcium phosphate phases by surface-analytical techniques

    Energy Technology Data Exchange (ETDEWEB)

    Kleine-Boymann, Matthias, E-mail: matthias.kleine-boymann@phys.chemie.uni-giessen.de; Rohnke, Marcus, E-mail: marcus.rohnke@phys.chemie.uni-giessen.de; Henss, Anja, E-mail: anja.henss@phys.chemie.uni-giessen.de; Peppler, Klaus, E-mail: klaus.peppler@phys.chemie.uni-giessen.de; Sann, Joachim, E-mail: joachim.sann@phys.chemie.uni-giessen.de; Janek, Juergen, E-mail: juergen.janek@phys.chemie.uni-giessen.de

    2014-08-01

    The spatially resolved phase identification of biologically relevant calcium phosphate phases (CPPs) in bone tissue is essential for the elucidation of bone remodeling mechanisms and for the diagnosis of bone diseases. Analytical methods with high spatial resolution for the discrimination between chemically quite close phases are rare. Therefore the applicability of state-of-the-art ToF-SIMS, XPS and EDX as chemically specific techniques was investigated. The eight CPPs hydroxyapatite (HAP), β-tricalcium phosphate (β-TCP), α-tricalcium phosphate (α-TCP), octacalcium phosphate (OCP), dicalcium phosphate dihydrate (DCPD), dicalcium phosphate (DCP), monocalcium phosphate (MCP) and amorphous calcium phosphate (ACP) were either commercial materials in high purity or synthesized by ourselves. The phase purity was proven by XRD analysis. All of the eight CPPs show different mass spectra and the phases can be discriminated by applying the principal component analysis method to the mass spectrometric data. The Ca/P ratios of all phosphates were determined by XPS and EDX. With both methods some CPPs can be distinguished, but the obtained Ca/P ratios deviate systematically from their theoretical values. It is necessary in any case to determine a calibration curve, respectively the ZAF values, from appropriate standards. In XPS also the O(1s)-satellite signals are correlated to the CPPs composition. Angle resolved and long-term XPS measurements of HAP clearly prove that there is no phosphate excess at the surface. Decomposition due to X-ray irradiation has not been observed.

  8. Controlled adsorption and release onto calcium phosphates materials and drug delivery applications

    Directory of Open Access Journals (Sweden)

    Barroug A.

    2013-11-01

    Full Text Available The adsorptive properties of synthetic calcium phosphates analogous to bone mineral were examined with respect to cisplatin and risedronate, two biological active drugs; the uptake and release experiments were carried out under various conditions in order to understand the basic mechanism of interaction. The effect of temperature and solution composition were highlighted and discussed. The adsorption results obtained for the therapeutic agents demonstrated that, depending on the conditions investigated (nature of the sorbent, concentration range, ionic composition, temperature…, the shape of the isotherms is of Freundlich or Langmuir type. The adsorption is described as an ion-exchange process in dilute solutions, while the interaction appears to be reactive for concentrated solutions (dissolution of mineral ions from the apatite substrate and formation of soluble calcium complex and/or precipitation of calcium salts involving sorbate molecules. The information gained on the surface reactivity of calcium phosphate were exploited to associate an antibiotic to calcium phosphate cements for drug delivery applications. The specimens were obtained by combination of calcium phosphate and calcium carbonate powders upon mixing with water. The physicochemical properties of the paste were altered by the drug loading method (in the liquid or solid phase. Thus, a dose-dependent effect was noticed for the paste setting time, hardening and the release process.

  9. A Raman spectroscopic study of the mono-hydrogen phosphate mineral dorfmanite Na 2(PO 3OH)·2H 2O and in comparison with brushite

    Science.gov (United States)

    Frost, Ray L.; Palmer, Sara J.; Xi, Yunfei

    2011-11-01

    Aspects of the molecular structure of the mineral dorfmanite Na 2(PO 3OH)·2H 2O were determined by Raman spectroscopy. The mineral originated from the Kedykverpakhk Mt., Lovozero, Kola Peninsula, Russia. Raman bands are assigned to the hydrogen phosphate units. The intense Raman band at 949 cm -1 and the less intense band at 866 cm -1 are assigned to the PO 3 and POH stretching vibrations. Bands at 991, 1066 and 1141 cm -1 are assigned to the ν3 antisymmetric stretching modes. Raman bands at 393, 413 and 448 cm -1 and 514, 541 and 570 cm -1 are attributed to the ν2 and ν4 bending modes of the HPO 4 units, respectively. Raman bands at 3373, 3443 and 3492 cm -1 are assigned to water stretching vibrations. POH stretching vibrations are identified by bands at 2904, 3080 and 3134 cm -1. Raman spectroscopy has proven very useful for the study of the structure of the mineral dorfmanite.

  10. Brushite-Forming Mg-, Zn- and Sr-Substituted Bone Cements for Clinical Applications

    Directory of Open Access Journals (Sweden)

    José M.F. Ferreira

    2010-01-01

    Full Text Available Calcium phosphate cements have been in clinical use for the last 10 years. Their most salient features include good biocompatibility, excellent bioactivity, self-setting characteristics, low setting temperature, adequate stiffness, and easy shaping to accomodate any complicated geometry. They are commonly used in filling bone defects and trauma surgeries as mouldable paste-like bone substitute materials. Substitution of trace elements, such as Mg, Sr and Zn ions, into the structure of calcium phosphates is the subject of widespread investigation nowadays, because of their impending role in the biological process. Subtle differences in composition and structure of these materials may have a profound effect on their in vivo behaviour. Therefore, the main goal of this paper is to provide a simple, but comprehensive overview of the present achievements relating to brushite-forming cements doped with Mg, Zn and Sr, and to identify new developments and trends. In particular, the influence of ionic substitution on the chemical, physical and biological properties of these materials is discussed.

  11. Is there a chemical interaction between calcium phosphates and organic compounds in the organic/inorganic composites?

    Energy Technology Data Exchange (ETDEWEB)

    Dorozhkin, S.V. [Research Inst. of Fertilisers, Moscow (Russian Federation)

    2001-07-01

    Solid composites of three biologically relevant calcium phosphates and hydroxypropylmethylcellulose (HPMC) were prepared at temperatures of 121 C. Properties of the composites obtained were studied by FTIR, X-ray diffraction, and SEM techniques. Special attention was devoted to seeking of a possible chemical interaction between the calcium phosphates and HPMC. No chemical interaction was found. Thus, HPMC was proven to have no influence on the chemical properties of calcium phosphates. (orig.)

  12. Pathogenic role of basic calcium phosphate crystals in destructive arthropathies.

    Directory of Open Access Journals (Sweden)

    Hang-Korng Ea

    Full Text Available basic calcium phosphate (BCP crystals are commonly found in osteoarthritis (OA and are associated with cartilage destruction. BCP crystals induce in vitro catabolic responses with the production of metalloproteases and inflammatory cytokines such as interleukin-1 (IL-1. In vivo, IL-1 production induced by BCP crystals is both dependant and independent of NLRP3 inflammasome. We aimed to clarify 1/ the role of BCP crystals in cartilage destruction and 2/ the role of IL-1 and NLRP3 inflammasome in cartilage degradation related to BCP crystals.synovial membranes isolated from OA knees were analysed by alizarin Red and FTIR. Pyrogen free BCP crystals were injected into right knees of WT, NLRP3 -/-, ASC -/-, IL-1α -/- and IL-1β-/- mice and PBS was injected into left knees. To assess the role of IL-1, WT mice were treated by intra-peritoneal injections of anakinra, the IL-1Ra recombinant protein, or PBS. Articular destruction was studied at d4, d17 and d30 assessing synovial inflammation, proteoglycan loss and chondrocyte apoptosis. BCP crystals were frequently found in OA synovial membranes including low grade OA. BCP crystals injected into murine knee joints provoked synovial inflammation characterized by synovial macrophage infiltration that persisted at day 30, cartilage degradation as evidenced by loss of proteoglycan staining by Safranin-O and concomitant expression of VDIPEN epitopes, and increased chondrocyte apoptosis. BCP crystal-induced synovitis was totally independent of IL-1α and IL-1β signalling and no alterations of inflammation were observed in mice deficient for components of the NLRP3-inflammasome, IL-1α or IL-1β. Similarly, treatment with anakinra did not prevent BCP crystal effects. In vitro, BCP crystals elicited enhanced transcription of matrix degrading and pro-inflammatory genes in macrophages.intra-articular BCP crystals can elicit synovial inflammation and cartilage degradation suggesting that BCP crystals have a direct

  13. Comparison of Calcium Phosphate and Zinc Oxide Nanoparticles as Dermal Penetration Enhancers for Albumin.

    Science.gov (United States)

    Shokri, Narges; Javar, H A

    2015-01-01

    Dermal drug delivery is highly preferred by patients due to its several advantages. Protein therapeutics have attracted huge attention recently. Since dermal delivery of proteins encounter problems, in this investigation, zinc oxide nanoparticles and calcium phosphate nanoparticles were compared as enhancers for dermal permeation of albumin. Albumin was applied simultaneously with zinc oxide nanoparticles or calcium phosphate nanoparticles on pieces of mouse skin. Skin permeation of albumin over time was determined using a diffusion cell. Skin distribution of the nanoparticles and albumin over time was determined by optical and fluorescence microscopy. Zinc oxide nanoparticles and calcium phosphate nanoparticles acted as enhancers for skin permeation of albumin. Cumulative permeated albumin in presence of zinc oxide nanoparticles after 0, 0.5, 1, 1.5 and 2 h, were 0±0, 11.7±3.3, 21.1±3.5, 40.2±3.6 and 40.2±3.6 mg, respectively and in presence of calcium phosphate nanoparticles were 0±0, 20.9±7.4, 33.8±5.5, 33.8±3.7 and 33.8±3.7 mg, respectively. After 0.5 h, little amount of albumin was permeated in presence of every kind of the nanoparticles. After 0.5 or 1 h, the permeated albumin in presence of calcium phosphate nanoparticles was more than that in presence of zinc oxide nanoparticles and after 1.5 h the permeated albumin in presence of zinc oxide nanoparticles was more than that in presence of calcium phosphate nanoparticles. Images of skin distribution of the two nanoparticles over time, were somewhat different and distribution of albumin correlated with the distribution of the nanoparticles alone. The profiles of albumin permeation (in presence of each of the nanoparticles) versus time was delayed and linear for both nanoparticles while the slope for calcium phosphate nanoparticles was higher than zinc oxide nanoparticles. The enhancer effect of zinc oxide nanoparticles was stronger while the enhancer effect of calcium phosphate nanoparticles was

  14. Antibody-conjugated soybean oil-filled calcium phosphate nanoshells for targetted delivery of hydrophobic molecules.

    Science.gov (United States)

    Schmidt, H T; Kroczynski, M; Maddox, J; Chen, Y; Josephs, R; Ostafin, A E

    2006-11-01

    Hollow calcium phosphate nanoparticles capable of encapsulating poorly water-soluble molecules were produced by self-assembly. Previously reported were solid calcium phosphate nanoparticles and water-filled calcium phosphate nanocapsules suited for encapsulating mostly hydrophilic, but not hydrophobic compounds. Here, calcium phosphate was deposited around 100 nm diameter, 1,2-dioleoyl-sn-glycero-3-phosphate stabilized soybean oil nanoemulsions using either calcium chloride or NaOH titrations to achieve shell thickness between 20-70 nm. The surface was functionalized with carboxylic acid via the addition of carboxyethylphosphonic acid to attach Molecular Probes AB-594C antibody using sulpho-n-hydroxysuccinimide and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride with an efficiency of approximately 70%, while retaining near complete antibody function. Hydrophobic pyrene was encapsulated with an efficiency of 95%, at concentrations much higher than its water solubility limit, and exhibited spectral features characteristic of a hydrophobic environment. These materials can be used in the targeted delivery of many useful, yet poorly water-soluble pharmaceutical and nutraceutical compounds.

  15. The effect of composition on mechanical properties of brushite cements.

    Science.gov (United States)

    Engstrand, Johanna; Persson, Cecilia; Engqvist, Håkan

    2014-01-01

    Due to a fast setting reaction, good biological properties, and easily available starting materials, there has been extensive research within the field of brushite cements as bone replacing material. However, the fast setting of brushite cement gives them intrinsically low mechanical properties due to the poor crystal compaction during setting. To improve this, many additives such as citric acid, pyrophosphates, and glycolic acid have been added to the cement paste to retard the crystal growth. Furthermore, the incorporation of a filler material could improve the mechanical properties when used in the correct amounts. In this study, the effect of the addition of the two retardants, disodium dihydrogen pyrophosphate and citric acid, together with the addition of β-TCP filler particles, on the mechanical properties of a brushite cement was investigated. The results showed that the addition of low amounts of a filler (up to 10%) can have large effects on the mechanical properties. Furthermore, the addition of citric acid to the liquid phase makes it possible to use lower liquid-to-powder ratios (L/P), which strongly affects the strength of the cements. The maximal compressive strength (41.8MPa) was found for a composition with a molar ratio of 45:55 between monocalcium phosphate monohydrate and beta-tricalcium phosphate, an L/P of 0.25ml/g and a citric acid concentration of 0.5M in the liquid phase.

  16. A comparative study of calcium phosphate formation on bioceramics in vitro and in vivo.

    Science.gov (United States)

    Xin, Renlong; Leng, Yang; Chen, Jiyong; Zhang, Qiyi

    2005-11-01

    Formation of calcium phosphate (Ca-P) on various bioceramic surfaces in simulated body fluid (SBF) and in rabbit muscle sites was investigated. The bioceramics were sintered porous solids, including bioglass, glass-ceramics, hydroxyapatite, alpha-tricalcium phosphate and beta-tricalcium phosphate. The ability of inducing Ca-P formation was compared among the bioceramics. The Ca-P crystal structures were identified using single-crystal diffraction patterns in transmission electron microscopy. The examination results show that ability of inducing Ca-P formation in SBF was similar among bioceramics, but considerably varied among bioceramics in vivo. Sintered beta-tricalcium phosphate exhibited a poor ability of inducing Ca-P formation both in vitro and in vivo. Octacalcium phosphate (OCP) formed on the surfaces of bioglass, A-W, hydroxyapatite and alpha-tricalcium phosphate in vitro and in vivo. Apatite formation in physiological environments cannot be confirmed as a common feature of bioceramics.

  17. FTIR/ATR study of protein adsorption and brushite transformation to hydroxyapatite.

    Science.gov (United States)

    Xie, Jing; Riley, Clyde; Kumar, Mukesh; Chittur, Krishnan

    2002-09-01

    Previous study has demonstrated that brushite (CaHPO4 x 2H2O), modified by partial potassium substitution for calcium, can transform quickly into hydroxyapatite (HA, Ca5(PO4)3OH) when exposed to aqueous salt solutions at room temperature. Analyses techniques used in those studies required sample retrieval from solution, which may alter the sample surface. In this work FTIR/ ATR was used in analysis, enabling in situ study of the transformation within the aqueous environment. To test the biocompatibility of this brushite, cellular response to the transformation needs to be understood. Cellular response was initiated by bovine serum albumin adsorption on the brushite surface. The response was studied by monitoring the conformation of the adsorbed protein, which is critical to cellular reaction. This required monitoring the brushite transformation and surface adsorbed protein conformation simultaneously which can be realized using FTIR/ATR. Based on band fitting and second derivative results from the spectra it was found that the conformation of the adsorbed BSA changes during the brushite transformation to HA. This study also demonstrated that the deposition of the brushite could be monitored in real time which offers the possibility for studying surface bonding during electrodeposition.

  18. Silver-doped calcium phosphate nanoparticles: synthesis, characterization, and toxic effects toward mammalian and prokaryotic cells.

    Science.gov (United States)

    Peetsch, Alexander; Greulich, Christina; Braun, Dieter; Stroetges, Christian; Rehage, Heinz; Siebers, Bettina; Köller, Manfred; Epple, Matthias

    2013-02-01

    Spherical silver-doped calcium phosphate nanoparticles were synthesized in a co-precipitation route from calcium nitrate/silver nitrate and ammonium phosphate in a continuous process and colloidally stabilized by carboxymethyl cellulose. Nanoparticles with 0.39 wt% silver content and a diameter of about 50-60 nm were obtained. The toxic effects toward mammalian and prokaryotic cells were determined by viability tests and determination of the minimal inhibitory and minimal bactericidal concentrations (MIC and MBC). Three mammalian cells lines, i.e. human mesenchymal stem cells (hMSC) and blood peripheral mononuclear cells (PBMC, monocytes and T-lymphocytes), and two prokaryotic strains, i.e. Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were used. Silver-doped calcium phosphate nanoparticles and silver acetate showed similar effect toward mammalian and prokaryotic cells with toxic silver concentrations in the range of 1-3 μg mL(-1).

  19. Calcium phosphate formation from sea urchin - (brissus latecarinatus via modified mechano-chemical (ultrasonic conversion method

    Directory of Open Access Journals (Sweden)

    R. Samur

    2013-07-01

    Full Text Available This study aims to produce apatite structures, such as hydroxyapatite (HA and fluorapatite (FA, from precursor calcium phosphates of biological origin, namely from sea urchin, with mechano-chemical stirring and hot-plating conversion method. The produced materials were heat treated at 800 °C for 4 hours. X-ray diffraction and scanning electron microscopy (SEM studies were conducted. Calcium phosphate phases were developed. The SEM images showed the formation of micro to nano-powders. The experimental results suggest that sea urchin, Brissus latecarinatus skeleton could be an alternative source for the production of various mono or biphasic calcium phosphates with simple and economic mechano-chemical (ultrasonic conversion method.

  20. Preparation and mechanism of calcium phosphate coatings on chemical modified carbon fibers by biomineralization

    Institute of Scientific and Technical Information of China (English)

    HUANG Su-ping; ZHOU Ke-chao; LI Zhi-you

    2008-01-01

    In order to prepare HA coatings on the carbon fibers, chemical modification and biomineralization processes were applied. The phase components, morphologies, and possible growth mechanism of calcium phosphate were studied by infrared spectroscopy(IR), X-ray diffractometry(XRD) and scanning electron microscopy(SEM). The results show that calcium phosphate coating on carbon fibers can be obtained by biomineralization. But the phase components and morphologies of calcium phosphate coatings are different due to different modification methods. Plate-like CaHPO4-2H2O (DCPD) crystals grow from one site of the active centre by HNO3 treatment. While on the para-aminobenzoic acid treated fibers, the coating is composed of nano-structural HA crystal homogeneously. This is because the -COOH functional groups of para-aminobenzoic acid graft on fibers, with negative charge and arranged structure, accelerating the HA crystal nucleation and crystallization on the carbon fibers.

  1. Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E., E-mail: w_prants@hotmail.com, E-mail: danielt_muller@yahoo.com.br, E-mail: sarahamindelima@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: gemelli@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Campus Universitario Prof. Avelino Marcante

    2009-07-01

    Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

  2. Synthesis and characterization of nanocomposite powders of calcium phosphate/titanium oxide for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Delima, S.A.; Camargo, N.H.A.; Souza, J.C.P.; Gemelli, E., E-mail: sarahamindelima@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: souzajulio@joinville.udesc.br, E-mail: gemelli@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas

    2009-07-01

    The nanostructured bioceramics of calcium phosphate are current themes of research and they are becoming important as bone matrix in regeneration of tissues in orthopedic and dental applications. Nanocomposite powders of calcium phosphate, reinforced with nanometric particles of titanium oxide, silica oxide and alumina oxid ealpha, are being widely studied because they offer new microstructures, nanostructures and interconnected microporosity with high superficial area of micropores that contribute to osteointegration and osteoinduction processes. This study is about the synthesis of nanocomposites powders of calcium phosphate reinforced with 1%, 2%, 3% and 5% in volume of titanium oxide and its characterization through the techniques of X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Differential Thermal Analysis (DTA), Thermogravimetry (TG) and Dilatometry. (author)

  3. Mechanical properties of calcium phosphate cements obtained by solution combustion synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Volkmer, Tiago M.; Barreiro, Oscar; Souza, Vania Caldas; Santos, Luis Alberto dos, E-mail: tiagovolkmer@gmail.com, E-mail: oscarbafer@hotmail.com, E-mail: vania.souza@ufrgs.br, E-mail: luis.santos@ufrgs.br [Universidade Federal do Rio Grande do Sul (UFRS), Porto Alegre, RS (Brazil). Laboratorio de Biomateriais

    2009-07-01

    Bioceramics based on calcium phosphates, especially hydroxyapatite and tricalcium phosphates (TCP) are the most used biomaterials as bone substitutes. The objective of this work is to evaluate the mechanical properties of α-tricalcium phosphate (α-TCP) synthesized by the solution combustion method. The solution combustion synthesis (SCS) can be considered as faster and simpler as other methods, furthermore it allows the obtainment of high purity α-TCP. In the calcium phosphates (CPC), α-TCP reacts with water forming needle like HA, which restrain the movement of grains, increasing mechanical resistance. In the present paper the influence of particle size on mechanical properties of α-TCP cements were evaluated. The α-TCP powder were characterized by XRD, TEM, BET and laser diffraction to asses particle size while the CPC bodies by SEM, Arquimedes method and compression tests. Increasing the milling time, the particle size decreases, resulting in samples with less porosity and consequently with higher compression resistance. (author)

  4. Encapsulation of plasmid DNA in calcium phosphate nanoparticles: stem cell uptake and gene transfer efficiency

    Directory of Open Access Journals (Sweden)

    Cao X

    2011-12-01

    Full Text Available Xia Cao*, Wenwen Deng*, Yuan Wei*, Weiyan Su, Yan Yang, Yawei Wei, Jiangnan Yu, Ximing XuDepartment of Pharmaceutics, School of Pharmacy, and Center for Nano Drug/Gene Delivery and Tissue Engineering, Jiangsu University, Jingkou District, Zhenjiang, People's Republic of China*These authors contributed equally to this workBackground: The purpose of this study was to develop calcium phosphate nanocomposite particles encapsulating plasmid DNA (CP-pDNA nanoparticles as a nonviral vector for gene delivery.Methods: CP-pDNA nanoparticles employing plasmid transforming growth factor beta 1 (TGF-β1 were prepared and characterized. The transfection efficiency and cell viability of the CP-pDNA nanoparticles were evaluated in mesenchymal stem cells, which were identified by immunofluorescence staining. Cytotoxicity of plasmid TGF-β1 and calcium phosphate to mesenchymal stem cells were evaluated by MTT assay.Results: The integrity of TGF-β1 encapsulated in the CP-pDNA nanoparticles was maintained. The well dispersed CP-pDNA nanoparticles exhibited an ultralow particle size (20–50 nm and significantly lower cytotoxicity than Lipofectamine™ 2000. Immunofluorescence staining revealed that the cultured cells in this study were probably mesenchymal stem cells. The cellular uptake and transfection efficiency of the CP-pDNA nanoparticles into the mesenchymal stem cells were higher than that of needle-like calcium phosphate nanoparticles and a standard calcium phosphate transfection kit. Furthermore, live cell imaging and confocal laser microscopy vividly showed the transportation process of the CP-pDNA nanoparticles in mesenchymal stem cells. The results of a cytotoxicity assay found that both plasmid TGF-β1 and calcium phosphate were not toxic to mesenchymal stem cells.Conclusion: CP-pDNA nanoparticles can be developed into an effective alternative as a nonviral gene delivery system that is highly efficient and has low cytotoxicity.Keywords: calcium

  5. Ossification Vesicles with Calcium Phosphate in the Eyes of the Insect Copium teucrii (Hemiptera: Tingidae

    Directory of Open Access Journals (Sweden)

    Javier Garcia-Guinea

    2011-01-01

    Full Text Available Arthropod eyes are built of repeating units named ommatidia. Each single ommatidium unit contains a cluster of photoreceptor cells surrounded by support cells and pigment cells. The insect Copium eye ommatidia include additional calcium-phosphate deposits, not described in insects to date, which can be examined today using a combined set of modern microscopy and spectroscopy techniques. Teucrium gnaphalodes L'Her plants, growing in central Spain, develop galls induced by Copium insects. A survey of C. teucrii adult specimens resulted in surprising environmental scanning electron microscopy (ESEM images, showing that their bright red eyes contain a calcium-phosphate mineralization. A complete survey of Copium eye specimens was performed by ESEM using energy-dispersive spectroscopy, backscattered electron detector and cathodoluminescence (CL probes, field emission scanning electron microscopy, micro-Raman spectroscopy, and confocal laser scanning microscopy in order to learn ommatidia features, such as chemical composition, molecular structure, cell membrane, and internal ommatidium eye fluids and calcium-phosphate distribution deposits. The CL panchromatic images distinguish between the calcium-phosphate ommatidium and calcium-phosphate setae, which are more apatite rich. They show Raman bands attributable to bone tissue apatite biomaterials, such as bone, collagen, lipids, and blood, i.e., peptides, amide-S, amide-II, amide-III, and cytochrome P-450scc. The chemical composition of both galls and leaves of T. gnaphalodes was determined by gas chromatography – mass spectrometry (GC-MS of their extracts. The spectrometric and microscopic images reveal that the calcium-phosphate mineralization is formed and constrained to Copium ommatidia, which are both matrix vesicles generating mixtures of apatite collagen and operational compound eyes of the insect.

  6. Vertical bone augmentation with granulated brushite cement set in glycolic acid.

    Science.gov (United States)

    Mariño, F Tamimi; Torres, J; Tresguerres, I; Jerez, L Blanco; Cabarcos, E López

    2007-04-01

    Brushite cements are a biocompatible materials that are resorbed in vivo. A new cement composed of a mixture of monocalcium phosphate (MCP) and beta-tricalcium phosphate (beta-TCP) that sets using glycolic acid (GA) was synthesized and characterized. After setting, the cement composition, derived from X-ray diffraction, was 83 wt % brushite and 17 wt % beta-TCP with an average brushite crystal size of about 2.6 +/- 1.4 microm. The cement has a diametral tensile strength of 2.9 +/- 0.7 MPa. Granules prepared from the set-cement were used as grafting material in bone defects on rabbit calvaria for evaluating in vivo its bone regeneration capacity. Considerable cement resorption, improvement in the bone mineral density, and bone neoformation was observed after 4 weeks of the granules' implantation.

  7. Biomimetic fabrication of calcium phosphate/chitosan nanohybrid composite in modified simulated body fluids

    Directory of Open Access Journals (Sweden)

    K. H. Park

    2017-01-01

    Full Text Available In this study, nucleation and growth of bone-like hydroxyapatite (HAp mineral in modified simulated body fluids (m-SBF were induced on chitosan (CS substrates, which were prepared by spin coating of chitosan on Ti substrate. The m-SBF showed a two fold increase in the concentrations of calcium and phosphate ions compared to SBF, and the post-NaOH treatment provided stabilization of the coatings. The calcium phosphate/chitosan composite prepared in m-SBF showed homogeneous distribution of approximately 350 nm-sized spherical clusters composed of octacalcium phosphate (OCP; Ca8H2(PO46·5H2O crystalline structure. Chitosan provided a control over the size of calcium phosphate prepared by immersion in m-SBF, and post-NaOH treatment supported the binding of calcium phosphate compound on the Ti surface. Post-NaOH treatment increased hydrophilicity and crystallinity of carbonate apatite, which increased its potential for biomedical application.

  8. Bioactivity evaluation of commercial calcium phosphate-based bioceramics for bone regeneration

    Energy Technology Data Exchange (ETDEWEB)

    Borrós, S.; Mas, A.

    2016-11-01

    Calcium phosphate-based bioceramics constitute a great promise for bone tissue engineering as they chemically resemble to mammalian bone and teeth. Their use is a viable alternative for bone regeneration as it avoids the use of autografts and allografts, which usually involves immunogenic reactions and patient’s discomfort. This work evolves around the study of the bioactivity potential of different commercially available bone substitutes based in calcium phosphate through the characterization of their ionic exchangeability when immersed in simulated body fluid (SBF). (Author)

  9. Synthesis and characterization of porous calcium phosphate; Sintesis y caracterizacion del fosfato de calcio poroso

    Energy Technology Data Exchange (ETDEWEB)

    Granados C, F.; Serrano G, J.; Bonifacio M, J. [ININ, 52750 La Marquesa, Estado de Mexico (Mexico)]. e-mail: fgc@nuclear.inin.mx

    2007-07-01

    The porous calcium phosphate was prepared by the continuous precipitation method using Ca(NO{sub 3}){sub 2}.4H{sub 2}O and NH{sub 4}H{sub 2}PO{sub 4} salts. The synthesized material was structurally and superficially characterized using the XRD, BET, IR TGA and SEM techniques. The obtained inorganic material was identified as calcium phosphate that presents a great specific area for what can be efficiently used as adsorbent material for adsorption studies in the radioactive wastes treatment present in aqueous solution. (Author)

  10. Effects of Additives on Sintering and Characterization of Calcium Phosphate Ceramics

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Calcium phosphate precursory powders containing Na and Mg have been prepared by the citric acid sol-gel combustion method. The elements of Na and Mg were introduced from component of CaO- P2O5-Na2 O-MgO. The effect of sintering additives on the phase composition was characterized by XRD. The effect of sintering additives on sintering of materials was also characterized by linear shrinkage, TEM and SEM. Finally the microstructure of porous calcium phosphate ceramic was determined by SEM.

  11. Serum Proteins Stabilized Calcium Phosphate Nanoparticles and Its Effect on Bel-7402 Cells

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Hydroxyapatite has a high affinity to biological macromolecules, especially to proteins. Bovine serum proteins were extracted to be used as stablizer to prepare calcium phosphate nanoparticles. 167.7 am and87.7 nm particles were respectively prepared by using bovine serum protein fractions at the concentration of 0.5mg/mL and 1.0 mg/mL. As the polysaccharide stabilized hydroxyapatite nanoparticles, the protein-stablized nanoparticles also inhibited the proliferation rate of Bel-7402 cells. It suggested that proteins could be applied to prepare calcium phosphate nanoparticles and it also has the anticancer effect.

  12. The effects of citric acid on the hydration of calcium phosphate cement

    Institute of Scientific and Technical Information of China (English)

    DAI Hong-lian; YAN Yu-hua; WANG You-fa; LI Shi-pu

    2001-01-01

    @@ INTRODUCTION Calcium phosphate cements (CPC) overcome the practical disadvantages of blocks or granulesl can be handled as a paste and sit in situ. Their structure and composition close to that of HAP make them biocompatible materials. 2 The conventional calcium phosphate cement had some problems such as long setting time (30~60 min) and low compressive strength, etc. In our system, an α-TCP/TTCP powder mixture was mixed with water containing citric acid to control the setting time and compressive strength. In this paper, the effects of various concentration citric acid solutions on the properties of the cement are reported.

  13. Treatment of post-orthodontic white spot lesions with casein phosphopeptide-stabilised amorphous calcium phosphate

    DEFF Research Database (Denmark)

    Bröchner, Ann; Christensen, Carsten; Kristensen, Bjarne;

    2010-01-01

    This study aims to investigate the effect of topical applications of 10% casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) on white spot lesions (WSL) detected after treatment with fixed orthodontic appliances. Sixty healthy adolescents with >/=1 clinically visible WSL at debonding were...... findings were largely reflected by the clinical scores. No side effects were reported. Topical treatment of white spot lesions after debonding of orthodontic appliances with a casein phosphopeptide-stabilised amorphous calcium phosphate agent resulted in significantly reduced fluorescence and a reduced...

  14. Correlation between calcium and phosphate levels to calculus accumulation on coronary heart disease patients

    Science.gov (United States)

    Cahaya, Cindy; Masulili, Sri Lelyati C.; Lessang, Robert; Radi, Basuni

    2017-02-01

    Coronary Artery Disease (CAD) or Coronary Heart Disease (CHD) is a disease that happened because of blood flow being blocked by atherosclerosis. Atherosclerosis is a process of hardening of the arteries which characterized by thickening and loss of elasticity of the intimal layer of vascular wall, by lipid deposit. Periodontitis is a chronic multifactorial inflammatory disease caused by microorganism and characterized by progressive destruction of the tooth supporting apparatus leading to tooth loss. Many studies use saliva as a valuable source for clinically information, as an asset for early diagnosis, prognostic and reviewer for pascatherapy status. Dental calculus had happened as a consequence of saliva supersaturation by calcium and phosphate. Salivary flow rate and its composition influence the formation of calculus. Increasing salivary calcium levels is characteristic of periodontitis patients. An important hipotesis in Cardiology is chronic infections contribute in atherosclerosis. Objective: To analyse the correlation between calcium and phosphate levels in saliva to calculus accumulation on CHD patients. Result: Correlation analysis between salivary calcium levels with calculus accumulation in patients with CHD and non-CHD showed no significant p value, p=0.59 and p=0.518. Correlation analysis between salivary phosphate levels and calculus accumulation showed no significant p value, p=0.836 for CHD patients and p=0.484 for non-CHD patients. Conclusion: There are no correlation between calcium levels and phosphate levels with calculus accumulation in CHD patients. Further research need to be done.

  15. Effect of rapidly resorbable calcium phosphates and a calcium phosphate bone cement on the expression of bone-related genes and proteins in vitro.

    Science.gov (United States)

    Knabe, C; Berger, G; Gildenhaar, R; Meyer, J; Howlett, C R; Markovic, B; Zreiqat, H

    2004-04-01

    The use of biodegradable bone substitutes is advantageous for alveolar ridge augmentation because it avoids second-site surgery for autograft harvesting. This study examines the effect of novel, rapidly resorbable calcium phosphates and a calcium phosphate bone cement on the expression of bone-related genes and proteins by human bone-derived cells (HBDCs) and compares this behavior to that of tricalciumphosphate (TCP). Test materials were alpha-TCP, two materials with a crystalline phase Ca(2)KNa(PO(4))(2) and with a small amorphous portion containing either magnesium potassium phosphate (material denominated GB14) or silica phosphate (material denominated GB9), and a calcium phosphate bone cement (material denominated Biocement D). HBDCs were grown on the substrata for 3, 7, 14, and 21 days, counted, and probed for various mRNAs and proteins (type I collagen, osteocalcin, osteopontin, osteonectin, alkaline phosphatase, and bone sialoprotein). All substrates supported continuous cellular growth for 21 days. In the presence of GB14 and Biocement D specimens cell proliferation was reduced and cell differentiation increased. At day 21, the greatest number of cells was found on GB9 expressing significantly higher levels of bone-related proteins than cells grown on all other surfaces. Because all novel materials facilitated the expression of the osteoblastic phenotype at least as much as TCP and the polystyrene control, these biomaterials can be regarded as excellent candidate bone substitute materials. GB9 induced the highest proliferation and cellular differentiation after 21 days of incubation, suggesting that this material may possess a higher potency for enhancing osteogenesis than TCP.

  16. Magnesium substitution in the structure of orthopedic nanoparticles: A comparison between amorphous magnesium phosphates, calcium magnesium phosphates, and hydroxyapatites.

    Science.gov (United States)

    Nabiyouni, Maryam; Ren, Yufu; Bhaduri, Sarit B

    2015-01-01

    As biocompatible materials, magnesium phosphates have received a lot of attention for orthopedic applications. During the last decade multiple studies have shown advantages for magnesium phosphate such as lack of cytotoxicity, biocompatibility, strong mechanical properties, and high biodegradability. The present study investigates the role of Mg(+2) and Ca(+2) ions in the structure of magnesium phosphate and calcium phosphate nanoparticles. To directly compare the effect of Mg(+2) and Ca(+2) ions on structure of nanoparticles and their biological behavior, three groups of nanoparticles including amorphous magnesium phosphates (AMPs) which release Mg(+2), calcium magnesium phosphates (CMPs) which release Mg(+2) and Ca(+2), and hydroxyapatites (HAs) which release Ca(+2) were studied. SEM, TEM, XRD, and FTIR were used to evaluate the morphology, crystallinity, and chemical properties of the particles. AMP particles were homogeneous nanospheres, whereas CMPs were combinations of heterogeneous nanorods and nanospheres, and HAs which contained heterogeneous nanosphere particles. Cell compatibility was monitored in all groups to determine the cytotoxicity effect of particles on studied MC3T3-E1 preosteoblasts. AMPs showed significantly higher attachment rate than the HAs after 1 day and both AMPs and CMPs showed significantly higher proliferation rate when compared to HAs after 7days. Gene expression level of osteoblastic markers ALP, COL I, OCN, OPN, RUNX2 were monitored and they were normalized to GAPDH housekeeping gene. Beta actin expression level was monitored as the second housekeeping gene to confirm the accuracy of results. In general, AMPs and CMPs showed higher expression level of osteoblastic genes after 7 days which can further confirm the stimulating role of Mg(+2) and Ca(+2) ions in increasing the proliferation rate, differentiation, and mineralization of MC3T3-E1 preosteoblasts.

  17. Combined effect of strontium and pyrophosphate on the properties of brushite cements.

    Science.gov (United States)

    Alkhraisat, M Hamdan; Mariño, F Tamimi; Rodríguez, C Rueda; Jerez, L Blanco; Cabarcos, E López

    2008-05-01

    In this study we report the synthesis of strontium-containing brushite cement with good cohesion and a diametral tensile strength (DTS) of 5 MPa. The cement powder, composed of beta-tricalcium phosphate (beta-TCP) and monocalcium phosphate, was adjusted by different concentrations of strontium and pyrophosphate ions. The cement liquid phase was 2M phosphoric acid solution. The cement cohesion and mechanical properties were measured after being aged in water for 24h at 37 degrees C. It was found that at low concentration both strontium and pyrophosphate ions inhibit the cement setting reaction. However, the final setting time was significantly reduced when SrCl2 increased from 5 to 10 wt.% at pyrophosphate concentrations equal to or higher than 2.16 wt.%. The incorporation of strontium ions did not increase the DTS of brushite cements significantly. In contrast, the addition of pyrophosphate ions did increase the DTS of brushite cements significantly. When both ions were added simultaneously, the brushite cement with a Sr2+ content of 5 wt.% had the highest DTS value. Nevertheless, the DTS values of Sr-containing cements were significantly reduced if the pyrophosphate concentration was higher than 2.16 wt.%. The Sr2+ ions had a negative effect on brushite cement cohesion, although the solid weight loss started to decrease at Sr2+ concentrations higher than 5 wt.%.

  18. Non-viral bone morphogenetic protein 2 transfection of rat dental pulp stem cells using calcium phosphate nanoparticles as carriers.

    NARCIS (Netherlands)

    Yang, X.; Walboomers, X.F.; Dolder, J. van den; Yang, F.; Bian, Z.; Fan, M.; Jansen, J.A.

    2008-01-01

    Calcium phosphate nanoparticles have shown potential as non-viral vectors for gene delivery. The aim of this study was to induce bone morphogenetic protein (Bmp)2 transfection in rat dental pulp stem cells using calcium phosphate nanoparticles as a gene vector and then to evaluate the efficiency and

  19. Effect of calcium phosphate crystals induced by uremic serum on calcification of human aortic smooth muscle cells

    Institute of Scientific and Technical Information of China (English)

    刘曜蓉

    2013-01-01

    Objective To investigate the impact of calcium phosphate crystals induced by uremic serum on calcification of human aortic smooth muscle cells (HASMCs) .Methods Uremic serum was incubated at 37℃for 3days.Calcium phosphate crystals and uremic supernatant were isolated from uremic serum by ultracentrifugation.

  20. Mapping calcium phosphate activated gene networks as a strategy for targeted osteoinduction of human progenitors.

    Science.gov (United States)

    Eyckmans, Jeroen; Roberts, Scott J; Bolander, Johanna; Schrooten, Jan; Chen, Christopher S; Luyten, Frank P

    2013-06-01

    Although calcium phosphate-containing biomaterials are promising scaffolds for bone regenerative strategies, the osteoinductive capacity of such materials is poorly understood. In this study, we investigated whether endogenous mechanisms of in vivo calcium phosphate-driven, ectopic bone formation could be identified and used to induce enhanced differentiation in vitro of the same progenitor population. To accomplish this, human periosteum derived cells (hPDCs) were seeded on hydroxyapatite/collagen scaffolds (calcium phosphate rich matrix or CPRM), or on decalcified scaffolds (calcium phosphate depleted matrix or CPDM), followed by subcutaneous implantation in nude mice to trigger ectopic bone formation. In this system, osteoblast differentiation occurred in CPRM scaffolds, but not in CPDM scaffolds. Gene expression was assessed by human full-genome microarray at 20 h after seeding, and 2, 8 and 18 days after implantation. In both matrices, implantation of the cell constructs triggered a similar gene expression cascade, however, gene expression dynamics progressed faster in CPRM scaffolds than in CPDM scaffolds. The difference in gene expression dynamics was associated with differential activation of hub genes and molecular signaling pathways related to calcium signaling (CREB), inflammation (TNFα, NFkB, and IL6) and bone development (TGFβ, β-catenin, BMP, EGF, and ERK signaling). Starting from this set of pathways, a growth factor cocktail was developed that robustly enhanced osteogenesis in vitro and in vivo. Taken together, our data demonstrate that through the identification and subsequent stimulation of genes, proteins and signaling pathways associated with calcium phosphate mediated osteoinduction, a focused approach to develop targeted differentiation protocols in adult progenitor cells can be achieved.

  1. Grafting cyclodextrins to calcium phosphate ceramics for biomedical applications

    DEFF Research Database (Denmark)

    Jacobsen, P.A.L.; Nielsen, J.L.; Juhl, M.V.

    2012-01-01

    The grafting of hydroxyapatite/beta-tricalcium phosphate with β-cyclodextrin was achieved using a two step reaction with (3-glycidyloxypropyl)trimethoxysilane as a linker. Firstly, the silane group was brought to react with the hydroxyl groups at the surface of the hydroxyapatite/beta-tricalcium ...

  2. Effects of Silicate, Phosphate, and Calcium on the Stability of Aldopentoses.

    Science.gov (United States)

    Nitta, Sakiko; Furukawa, Yoshihiro; Kakegawa, Takeshi

    2016-06-01

    Ribose is an important constituent of RNA: ribose connects RNA bases and forms a strand of sugar phosphates. Accumulation of ribose on prebiotic Earth was difficult because of its low stability. Improvement in the yield of ribose by the introduction of borate or silicate in a formose-like reaction has been proposed. The effects of borates have been further analyzed and confirmed in subsequent studies. Nonetheless, the effects of silicates and phosphates remain unclear. In the present study, we incubated aldopentoses in a highly alkaline aqueous solution at a moderate temperature to determine the effects of silicate or phosphate on the degradation rates of ribose and its isomeric aldopentoses. The formation of a complex of silicate (or phosphate) with ribose was also analyzed in experiments with (29)Si and (31)P nuclear magnetic resonance (NMR). We found that silicate or phosphate complexes of ribose were not detectable under our experimental conditions. The stability of ribose and lyxose improved after addition of 40-fold molar excess (relative to a pentose) of sodium silicate or sodium phosphate to the alkaline solution. The stability was not improved further when an 80-fold molar excess of sodium silicate or sodium phosphate was added. Calcium was removed from these solutions by precipitation of calcium salts. The drop in Ca(2+) concentration might have improved the stability of ribose and lyxose, which are susceptible to aldol addition. The improvement of ribose stability by the removal of Ca(2+) and by addition of silicate or phosphate was far smaller than the improvement by borate. Furthermore, all aldopentoses showed similar stability in silicate- and phosphate-containing solutions. These results clearly show that selective stabilization of ribose by borate cannot be replaced by the effects of silicate or phosphate; this finding points to the importance of borate in prebiotic RNA formation.

  3. The determination of calcium in phosphate, carbonate, and silicate rocks by flame photometer

    Science.gov (United States)

    Kramer, Henry

    1956-01-01

    A method has been developed for the determination of calcium in phosphate, carbonate, and silicate rocks using the Beckman flame photometer, with photomultiplier attachement. The sample is dissolved in hydrofluoric, nitric, and perchloric acids, the hydrofluoric and nitric acids are expelled, a radiation buffer consisting of aluminum, magnesium, iron, sodium, potassium, phosphoric acid, and nitric acid is added, and the solution is atomized in an oxy-hydrogen flame with an instrument setting of 554 mµ. Measurements are made by comparison against calcium standards, prepared in the same manner, in the 0 to 50 ppm range. The suppression of calcium emission by aluminum and phosphate was overcome by the addition of a large excess of magnesium. This addition almost completely restores the standard curve obtained from a solution of calcium nitrate. Interference was noted when the iron concentration in the aspirated solution (including the iron from the buffer) exceeded 100 ppm iron. Other common rock-forming elements did not interfere. The results obtained by this procedure are within ± 2 percent of the calcium oxide values obtained by other methods in the range 1 to 95 percent calcium oxide. In the 0 to 1 percent calcium oxide range the method compares favorably with standard methods.

  4. Dietary Calcium Phosphate Stimulates Intestinal Lactobacilli and decreases the severity of a salmonella infection in rats

    NARCIS (Netherlands)

    Bovee-Oudenhoven, I.M.; Wissink, M.L.; Wouters, J.T.; Meer, van der R.

    1999-01-01

    We have shown recently that dietary calcium phosphate (CaPi) has a trophic effect on the intestinal microflora and strongly protects against salmonella infection. It was speculated that precipitation by CaPi of intestinal surfactants, such as bile acids and fatty acids, reduced the cytotoxicity of i

  5. Calcium phosphate coating on magnesium alloy by biomimetic method :Investigation of morphology ,composition and formation process

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Magnesium alloy has similar mechanical properties with natural bone and can degrade via corrosion in the electrolytic environment of the human body.Calcium phosphate has been proven to possess bioactivity and bone inductivity.In order to integrate both advantages,calcium phosphate coating was fabricated on magnesium alloy by a biomimetic method.Supersaturated calcification solutions (SCSs) with different Ca/P ratio and C1- concentration were used as mimetic solutions.The morphology,composition and formation process of the coating were studied with scanning electron microscopy (SEM),energy dispersive spectrometer (EDS),Fourier transformed infrared spectroscopy (FTIR) and X-ray diffraction (XRD).The results show that a uniform calcium phosphate coating was observed on magnesium alloy,the properties of which could be adjusted by the SCSs with different Ca/P ratio.The formation process of the coating was explored by immersing magnesium alloy in SCSs with different Cl- concentration which could adjust the hydrogen production.According to SEM results,the hydrogen bubbles were associated with the formation of grass-like and flower-like coating morphologies.In conclusion,the biomimetic method was effective to form calcium phosphate coating on magnesium alloy and the morphology and composition of the coating could be accommodated by the Ca/P ratio and Cl- concentration in SCSs.

  6. FORMATION OF PHOSPHATE-CONTAINING CALCIUM-FLUORIDE AT THE EXPENSE OF ENAMEL, HYDROXYAPATITE AND FLUORAPATITE

    NARCIS (Netherlands)

    CHRISTOFFERSEN, J; CHRISTOFFERSEN, MR; ARENDS, J; LEONARDSEN, ES

    1995-01-01

    During the caries process complex reactions involving calcium, phosphate, hydrogen and fluoride ions as main species take place. In this study the precipitation and dissolution reactions occurring in suspensions of enamel, hydroxyapatite (HAP) and fluorapatite (FAP) on addition of fluoride were inve

  7. Controlling surface microstructure of calcium phosphate ceramic from random to custom-design

    NARCIS (Netherlands)

    Wang, Liao; Luo, Xiaoman; Barbieri, D.; Bao, Chongyun; Yuan, Huipin

    2014-01-01

    Calcium phosphate ceramics have long been studied as bone graft substitutes due to their similarity with the mineral constitute of bone and teeth, excellent biocompatibility and bioactivity. Chemical composition, macrostructure and surface microstructure are believed to be important for the bone for

  8. A study about some phosphate derivatives as inhibitors of calcium oxalate crystal growth

    Science.gov (United States)

    Grases, F.; March, P.

    1989-08-01

    The kinetic of crystal growth of calcium oxalate monohydrate seed crystals were investigated potentiometrically in the presence of several phosphate derivatives, D-fructose-1,6-diphosphate, pyrophosphate, methylene diphosphonate and phytate, and it was found that in some cases they strongly inhibited crystal growth. The inhibitory action of the different substances assayed was comparatively evaluated.

  9. Cost containment using cysteine HCl acidification to increase calcium/phosphate solubility in hyperalimentation solutions.

    Science.gov (United States)

    Schmidt, G L; Baumgartner, T G; Fischlschweiger, W; Sitren, H S; Thakker, K M; Cerda, J J

    1986-01-01

    The purpose of this study was to determine if (1) the calcium/phosphate insoluble product was inversely related to pH [when cysteine HC1 (CH) was added as neonatal supplementation at 0.5 mM/kg/day to hyperalimentation (HAL) solutions] and (2) the potential cost savings to the hospital. The pH of the HAL solutions was adjusted by adding various amounts of CH to the HAL solution. HAL solutions containing 27 mEq of calcium/liter and 30 mEq (15 mM) of phosphate/liter were compounded. Ten-milliliter aliquots were analyzed at 0, 12, 24, and 48 hr. All samples (n = 56) were filtered (0.22 mu), viewed with 7-10,000 X magnification scanning electron microscopy, and qualitatively analyzed with a Philips Energy Dispersive X-Ray Analysis System equipped with a SW9100 Microprocessor. Calcium/phosphate insoluble product was present in the 0-, 12-, 24-, and 48-hr samples from the CH-free solutions. The solutions containing 759 mg (4.17 mM)/liter of CH however, remained free of precipitant. This investigation demonstrated that addition of CH to HAL can foster significant cost containment (projected $82,000/yr tangible hospital savings) by the elimination of current calcium/phosphate separation procedures for neonates on parenteral nutrition.

  10. Bioactivity and Surface Reactivity of RF-sputtered Calcium Phosphate Thin Films

    NARCIS (Netherlands)

    Wal, Edwin van der

    2003-01-01

    Calcium phosphates (CaP) are known to be bioactive, i.e. able to bond to bone. This makes CaPs very suitable to be aplied as thin coatings on bone-implants. In this work we studied the physicochemical behaviour of CaP coatings applied with radio frequency (RF) magnetron sputtering, a deposition tech

  11. Dense and porous titanium substrates with a biomimetic calcium phosphate coating

    Energy Technology Data Exchange (ETDEWEB)

    Ribeiro, A.A., E-mail: aantunesr@yahoo.com.br [Powder Technology Laboratory, Materials Processing and Characterization Division, National Institute of Technology, No. 82 Venezuela Avenue, Room 602, 20081-312 Rio de Janeiro, RJ (Brazil); Balestra, R.M. [Powder Technology Laboratory, Materials Processing and Characterization Division, National Institute of Technology, No. 82 Venezuela Avenue, Room 602, 20081-312 Rio de Janeiro, RJ (Brazil); Rocha, M.N. [Metallurgical and Materials Engineering Program, COPPE, Federal University of Rio de Janeiro, P.O. Box 68505, 21941-972 Rio de Janeiro, RJ (Brazil); Peripolli, S.B. [Materials Metrology Division, National Institute of Metrology, Normalization and Quality, No. 50 Nossa Senhora das Gracas Street, Building 3, 25250-020 Duque de Caxias, RJ (Brazil); Andrade, M.C. [Polytechnic Institute of Rio de Janeiro, Rio de Janeiro State University, s/n, Alberto Rangel Street, 28630-050 Nova Friburgo, RJ (Brazil); Pereira, L.C. [Metallurgical and Materials Engineering Program, COPPE, Federal University of Rio de Janeiro, P.O. Box 68505, 21941-972 Rio de Janeiro, RJ (Brazil); Oliveira, M.V. [Powder Technology Laboratory, Materials Processing and Characterization Division, National Institute of Technology, No. 82 Venezuela Avenue, Room 602, 20081-312 Rio de Janeiro, RJ (Brazil)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer A biomimetic coating method with simplified solution is proposed. Black-Right-Pointing-Pointer Titanium substrates are submitted to chemical and heat treatments. Black-Right-Pointing-Pointer Titanium substrates are coated with biocompatible calcium phosphate phases. Black-Right-Pointing-Pointer The simplified solution shows potential to be applied as a coating technique. - Abstract: The present work studied a biomimetic method using a simplified solution (SS) with calcium and phosphorus ions for coating titanium substrates, in order to improve their bioactivity. Commercially pure titanium dense sheet, microporous and macroporous titanium samples, both produced by powder metallurgy, were treated in NaOH solution followed by heat-treating and immersed in SS for 7, 14 or 21 days. The samples characterization was performed by quantitative metallographic analysis, confocal scanning optical microscopy, scanning electron microscopy, energy dispersive spectroscopy and low angle X-ray diffraction. The results showed coatings with calcium phosphate precipitation in all samples, with globular or plate-like morphology, typical of hydroxyapatite and octacalcium phosphate, respectively, indicating that the solution (SS) has potential for coating titanium substrates. In addition, the different surfaces of substrates had an effect on the formed calcium phosphate phase and thickness of coatings, depending on the substrate type and imersion time in the simplified solution.

  12. Trabecular bone response to injectable calcium phosphate (Ca-P) cement.

    NARCIS (Netherlands)

    Ooms, E.M.; Wolke, J.G.C.; Waerden, J.P.C.M. van der; Jansen, J.A.

    2002-01-01

    The aim of this study was to investigate the physicochemical, biological, and handling properties of a new developed calcium phosphate (Ca-P) cement when implanted in trabecular bone. Ca-P cement consisting of a powder and a liquid phase was implanted as a paste into femoral trabecular bone of goats

  13. PLGA microsphere/calcium phosphate cement composites for tissue engineering: in vitro release and degradation characteristics.

    NARCIS (Netherlands)

    Habraken, W.J.E.M.; Wolke, J.G.C.; Mikos, A.G.; Jansen, J.A.

    2008-01-01

    Bone cements with biodegradable poly(lactic-co-glycolic acid) (PLGA) microspheres have already been proven to provide a macroporous calcium phosphate cement (CPC) during in situ microsphere degradation. Furthermore, in vitro/in vivo release studies with these PLGA microsphere/CPC composites (PLGA/CP

  14. Incorporation of biodegradable electrospun fibers into calcium phosphate cement for bone regeneration.

    NARCIS (Netherlands)

    Zuo, Y.; Yang, F.; Wolke, J.G.C.; Li, Yubao; Jansen, J.A.

    2010-01-01

    Inherent brittleness and slow degradation are the major drawbacks for the use of calcium phosphate cements (CPCs). To address these issues, biodegradable ultrafine fibers were incorporated into the CPC in this study. Four types of fibers made of poly(epsilon-caprolactone) (PCL) (PCL12: 1.1 microm, P

  15. Analysis of integrin expression in U2OS cells cultured on various calcium phosphate ceramic substrates.

    NARCIS (Netherlands)

    Ruijter, J.E. de; Brugge, P.J. ter; Dieudonne, S.C.; Vliet, S.J. van; Torensma, R.; Jansen, J.A.

    2001-01-01

    Earlier we observed that calcium phosphate (Ca-P)-coated implant substrates stimulated the differentiation of osteoblast-like cells compared to uncoated substrates. This suggests that this difference in osteogenic induction is due to the chemical composition of the substratum. We hypothesized that C

  16. Injectable thermosensitive hydrogel composite with surface-functionalized calcium phosphate as raw materials

    Directory of Open Access Journals (Sweden)

    Fan RR

    2014-01-01

    Full Text Available RangRang Fan,1 XiaoHui Deng,2 LiangXue Zhou,1 Xiang Gao,1 Min Fan,1 YueLong Wang,1 Gang Guo11State Key Laboratory of Biotherapy and Cancer Center, Department of Neurosurgery, West China Hospital, West China Medical School, Sichuan University, Chengdu, 2Department of Human Anatomy, Xinxiang Medical University, Xinxiang, People's Republic of ChinaAbstract: In this study, L-lactide was used to modify the tricalcium phosphate (β-TCP and tetracalcium phosphate (TTCP surface which can form functionalized poly(l-lactic acid (PLLA-grafted β-TCP (g-β-TCP and PLLA-grafted TTCP (g-TTCP particles. The g-β-TCP and g-TTCP obtained were incorporated into a PEG-PCL-PEG (PECE matrix to prepare injectable thermosensitive hydrogel composites. The morphology of the hydrogel composites showed that the g-β-TCP and g-TTCP particles dispersed homogeneously into the polymer matrix, and each hydrogel composite had a three-dimensional network structure. Rheologic analysis showed that the composite had good thermosensitivity. Changes in calcium concentration and pH in simulated body fluid solutions confirmed the feasibility of surface-functionalized calcium phosphate for controlled release of calcium. All the results indicate that g-β-TCP/PECE and g-TTCP/PECE hydrogels might be a promising protocol for tissue engineering.Keywords: injectable, thermosensitivity, surface functionalization, calcium phosphate, biocompatibility

  17. Ectopic osteoid and bone formation by three calcium-phosphate ceramics in rats, rabbits and dogs

    NARCIS (Netherlands)

    Wang, Liao; Zhang, B.; Bao, C.; Habibovic, P.; Hu, J.; Zhang, Xingdong

    2014-01-01

    Calcium phosphate ceramics with specific physicochemical properties have been shown to induce de novo bone formation upon ectopic implantation in a number of animal models. In this study we explored the influence of physicochemical properties as well as the animal species on material-induced ectopic

  18. In vivo performance of microstructured calcium phosphate formulated in novel water-free carriers

    NARCIS (Netherlands)

    Davison, N.L.; Yuan, H.; Bruijn, de J.D.; Barrere-de Groot, F.YF.

    2012-01-01

    Osteoinductive calcium phosphate (CaP) ceramics can be combined with polymeric carriers to make shapeable bone substitutes as an alternative to autologous bone; however, carriers containing water may degrade the ceramic surface microstructure, which is crucial to bone formation. In this study five n

  19. Novel tea polyphenol-modified calcium phosphate nanoparticle and its remineralization potential

    NARCIS (Netherlands)

    He, L.; Deng, D.; Zhou, X.; Cheng, L.; ten Cate, J.M.; Li, J.; Li, X.; Crielaard, W.

    2015-01-01

    Tea polyphenols (TP) are not only potent antimicrobial and antioxidant agents but also effective modifiers in the formation of nanosized crystals. Since nano-hydroxyapatite (n-HA) is known to enhance remineralization of dental hard tissue, our aims were to synthesize nanosized calcium phosphate part

  20. Biocompatibility and degradation of poly(DL-lactic-co-glycolic acid)/calcium phosphate cement composites

    NARCIS (Netherlands)

    Ruhe, P.Q.; Hedberg, E.L.; Padron, N.T.; Spauwen, P.H.M.; Jansen, J.A.; Mikos, A.G.

    2005-01-01

    Injectable calcium phosphate (Ca-P) cement materials exhibit favorable osteocompatible behavior but are resorbed slowly because of a lack of a bone ingrowth-enabling macroporosity. In this study, poly(DL-lactic-co-glycolic acid) (PLGA) microparticles (average size 66 +/- 25 microm) were incorporated

  1. Introduction of enzymatically degradable poly(trimethylene carbonate) microspheres into an injectable calcium phosphate cement

    NARCIS (Netherlands)

    Habraken, Wouter J. E. M.; Zhang, Zheng; Wolke, Joop G. C.; Grijpma, Dirk W.; Mikos, Antonios G.; Feijen, Jan; Jansen, John A.

    2008-01-01

    Poly(trimethylene carbonate) (PTMC) is an enzymatically degradable polyester with rubber-like properties. Introduction of this polymer into an injectable calcium phosphate bone cement can therefore be used to introduce macroporosity into the cement for tissue engineering purposes as well as to impro

  2. Injectable PLGA microsphere/calcium phosphate cements: physical properties and degradation characteristics.

    NARCIS (Netherlands)

    Habraken, W.J.E.M.; Wolke, J.G.C.; Mikos, A.G.; Jansen, J.A.

    2006-01-01

    Calcium phosphate (CaP) cements show an excellent biocompatibility and often have a high mechanical strength, but in general degrade relatively slow. To increase degradation rates, macropores can be introduced into the cement, e.g., by the inclusion of biodegradable microspheres into the cement. The

  3. Introduction of enzymatically degradable poly(trimethylene carbonate) microspheres into an injectable calcium phosphate cement.

    NARCIS (Netherlands)

    Habraken, W.J.E.M.; Zhang, Z.; Wolke, J.G.C.; Grijpma, D.W.; Mikos, A.G.; Feijen, J.; Jansen, J.A.

    2008-01-01

    Poly(trimethylene carbonate) (PTMC) is an enzymatically degradable polyester with rubber-like properties. Introduction of this polymer into an injectable calcium phosphate bone cement can therefore be used to introduce macroporosity into the cement for tissue engineering purposes as well as to impro

  4. Influence of surface microstructure and chemistry on osteoinduction and osteoclastogenesis by biphasic calcium phosphate discs.

    NARCIS (Netherlands)

    Davison, N.L.; Su, J.; Yuan, H.; Beucken, J.J.J.P van den; Bruijn, J.D. de; rrere-de Groot, F. Ba

    2015-01-01

    It has been reported that surface microstructural dimensions can influence the osteoinductivity of calcium phosphates (CaPs), and osteoclasts may play a role in this process. We hypothesised that surface structural dimensions of

  5. Processing and properties of calcium phosphates bioceramics by hot isostatic pressing

    Directory of Open Access Journals (Sweden)

    Boilet Laurent

    2013-11-01

    Full Text Available Stoichiometric β-tricalcium phosphate (β-TCP, hydroxyapatite (HA and biphasic calcium phosphate (TCP/HA 60/40 %wt, BCP40 powders were synthesized by chemical precipitation of aqueous solutions of diammonium phosphate and calcium nitrate. After a calcination treatment and a milling step, powders were shaped by slip-casting. The sintering temperature effect on the density and the average grain size was investigated. By natural sintering, densities between 98 and 99.8% were obtained. Hot Isostatic Pressing (HIP treatment was carried out after a pre-sintering of these materials. Transparent or translucent samples were obtained, indicating a relative density very close to the theoretical value (>99.9%. Mechanical properties (three-point bending strength, fracture toughness, Young's modulus and Vickers hardness were measured on hipped materials with similar grain size (∼0.7μm.

  6. Calcium phosphate holmium-166 ceramic to addition in bone cement: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Donanzam, Blanda A.; Campos, Tarcisio P.R., E-mail: campos@nuclear.ufmg.b [Universidade do Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Escola de Engenharia. Dept. de Engenharia Nuclear; Dalmazio, Ilza; Valente, Eduardo S., E-mail: id@cdtn.b, E-mail: valente@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2011-07-01

    Spine metastases are a common and painful complication of cancer. The treatment often consists of bone cement injection (vertebroplasty or kyphoplasty) within vertebral body for vertebrae stabilization, followed by external beam radiation therapy. Recently, researchers introduced the concept of radioactive bone cement for spine tumors therapy. Then, investigations about bioactive and radioactive materials became interesting. In this study, we present the synthesis of calcium phosphate incorporated holmium (CaP-Ho) via sol-gel technique, and its characterization by XRD, FT-IR, NA and SEM. Results showed a multiphasic bioceramic composed mainly of hydroxyapatite, {beta}-tricalcium phosphate, holmium phosphate and traces of calcium pyrophosphate. Furthermore, the nuclide Ho-166 was the major radioisotope produced. Despite that, the radioactive bioceramic CaP-{sup 166}Ho must be investigated in clinical trials to assure its efficacy and safety on spine tumors treatment (author)

  7. A construction of novel iron-foam-based calcium phosphate/chitosan coating biodegradable scaffold material.

    Science.gov (United States)

    Wen, Zhaohui; Zhang, Liming; Chen, Chao; Liu, Yibo; Wu, Changjun; Dai, Changsong

    2013-04-01

    Slow corrosion rate and poor bioactivity restrict iron-based implants in biomedical application. In this study, we design a new iron-foam-based calcium phosphate/chitosan coating biodegradable composites offering a priority mechanical and bioactive property for bone tissue engineering through electrophoretic deposition (EPD) followed by a conversion process into a phosphate buffer solution (PBS). Tensile test results showed that the mechanical property of iron foam could be regulated through altering the construction of polyurethane foam. The priority coatings were deposited from 40% nano hydroxyapatite (nHA)/ethanol suspension mixed with 60% nHA/chitosan-acetic acid aqueous solution. In vitro immersion test showed that oxidation-iron foam as the matrix decreased the amount of iron implanted and had not influence on the bioactivity of this implant, obviously. So, this method could also be a promising method for the preparation of a new calcium phosphate/chitosan coating on foam construction.

  8. Phase stability of silver particles embedded calcium phosphate bioceramics

    Indian Academy of Sciences (India)

    Brajendra Singh; Samayendra Kumar; Naresh Saha; Bikramjit Basu; Rajeev Gupta

    2015-04-01

    In this paper, we report the compositional variation-dependent phase stability of hydroxyapatite (Ca10(PO4)6(OH)2) on doping with silver. The transformation of hydroxyapatite to (/) tricalcium phosphate phases during sintering has been explored using Raman spectroscopy and X-ray diffraction techniques. The optical absorption spectroscopy analysis reveals the presence of Ag+ ions at low doping levels. As the doping increases, abundance of Ag particles is enhanced.

  9. Modelling biological and chemically induced precipitation of calcium phosphate in enhanced biological phosphorus removal systems.

    Science.gov (United States)

    Barat, R; Montoya, T; Seco, A; Ferrer, J

    2011-06-01

    The biologically induced precipitation processes can be important in wastewater treatment, in particular treating raw wastewater with high calcium concentration combined with Enhanced Biological Phosphorus Removal. Currently, there is little information and experience in modelling jointly biological and chemical processes. This paper presents a calcium phosphate precipitation model and its inclusion in the Activated Sludge Model No 2d (ASM2d). The proposed precipitation model considers that aqueous phase reactions quickly achieve the chemical equilibrium and that aqueous-solid change is kinetically governed. The model was calibrated using data from four experiments in a Sequencing Batch Reactor (SBR) operated for EBPR and finally validated with two experiments. The precipitation model proposed was able to reproduce the dynamics of amorphous calcium phosphate (ACP) formation and later crystallization to hydroxyapatite (HAP) under different scenarios. The model successfully characterised the EBPR performance of the SBR, including the biological, physical and chemical processes.

  10. A novel biodegradable nicotinic acid/calcium phosphate composite coating on Mg-3Zn alloy

    Energy Technology Data Exchange (ETDEWEB)

    Song, Yingwei, E-mail: ywsong@imr.ac.cn; Shan, Dayong; Han, En-Hou

    2013-01-01

    A novel biodegradable composite coating is prepared to reduce the biodegradation rate of Mg-3Zn alloy. The Mg-3Zn substrate is first immersed into 0.02 mol L{sup -1} nicotinic acid (NA) solution, named as vitamin B{sub 3}, to obtain a pretreatment film, and then the electrodeposition of calcium phosphate coating with ultrasonic agitation is carried out on the NA pretreatment film to obtain a NA/calcium phosphate composite coating. Surface morphology is observed by scanning electron microscopy (SEM). Chemical composition is determined by X-ray diffraction (XRD) and EDX. Protection property of the coatings is evaluated by electrochemical tests. The biodegradable behavior is investigated by immersion tests. The results indicate that a thin but compact bottom layer can be obtained by NA pretreatment. The electrodeposition calcium phosphate coating consists of many flake particles and ultrasonic agitation can greatly improve the compactness of the coating. The composite coating is biodegradable and can reduce the biodegradation rate of Mg alloys in stimulated body fluid (SBF) for twenty times. The biodegradation process of the composite coating can be attributed to the gradual dissolution of the flake particles into chippings. - Highlights: Black-Right-Pointing-Pointer NA/calcium phosphate composite coating is prepared to protect Mg-3Zn alloy implant. Black-Right-Pointing-Pointer Nicotinic acid (vitamin B{sub 3}) is available to obtain a protective bottom film. Black-Right-Pointing-Pointer Ultrasonic agitation greatly improves the compactness of calcium phosphate coating. Black-Right-Pointing-Pointer The composite coating can reduce the biodegradation rate of Mg-3Zn twenty times. Black-Right-Pointing-Pointer The composite coating is biodegraded by the dissolution of flakes into chippings.

  11. Extrusion-based, three-dimensional printing of calcium-phosphate scaffolds

    Science.gov (United States)

    Witek, Lukasz

    Small or large bone defects, can occur due to a variety of reasons: congenital disorders, infections, tumors, or traumas which can lead to significant disabilities. There is an assortment of bone grafting procedures, each having their own respective advantages and disadvantages and exhibiting certain essential characteristics. Among the available grafts, autogenous (autograft), allograft, xenograft, and alloplasts, all exhibit a minimum of two-thirds of the essential characteristics and have been proven useful in fully or partially repairing skeletal defects. However, different host-to-grafting material responses have been reported and should be taken into consideration when determining treatment options. A large range of physical and chemical properties can be achieved with calcium phosphate based materials, which possess two of the ideal characteristics for grafting procedures: osteoconduction and osseointegration. Calcium phosphate based scaffolds composed of hydroxyapatite (HA), beta-tri-calcium phosphate (beta-TCP), or a combination of both (HA/beta-TCP) were investigated as materials for three-dimensional printing process to create layer-by-layer structures for use as bone regeneration scaffolds. Different calcium-phosphate phases will result in different degrees of in vivo dissolution and/or cell-mediated resorption. There has been a growing interest in BCP because it has been shown that this material improves the formation of new bone inside the implanted scaffold. The literature indicates that the faster dissolution rate of ?-TCP would be greatly responsible of this enhancement. However, in vitro tests indicate that fast dissolution can decrease the mechanical strength of BCP scaffolds. Furthermore, studies reported that HA has higher mechanical strength and lower degradation rate than beta-TCP. Therefore, the HA/beta-TCP ratio is a key parameter controlling the performance of the scaffold for bone repair applications, since it determines degradation rate

  12. Kinetic study of the setting reaction of a calcium phosphate bone cement.

    Science.gov (United States)

    Fernández, E; Ginebra, M P; Boltong, M G; Driessens, F C; Ginebra, J; De Maeyer, E A; Verbeeck, R M; Planell, J A

    1996-11-01

    The setting reaction of a calcium phosphate bone cement consisting of a mixture of 63.2 wt % alpha-tertiary calcium phosphate (TCP)[alpha-Ca3(PO4)2], 27.7 wt % dicalcium phosphate (DCP) (CaHPO4), and 9.1 wt % of precipitated hydroxyapatite [(PHA) used as seed material] was investigated. The cement samples were prepared at a liquid-to-powder ratio of: L/P = 0.30 ml/g. Bi-distilled water was used as liquid solution. After mixing the powder and liquid, some samples were molded and aged in Ringer's solution at 37 degrees C. At fixed time intervals they were unmolded and then immediately frozen in liquid nitrogen at a temperature of TN = -196 degrees C, lyofilized, and examined by X-ray diffraction as powder samples. The compressive strength versus time was also measured in setting samples of this calcium phosphate bone cement. The crystal entanglement morphology was examined by scanning electron microscopy. The results showed that: 1) alpha-TCP reacted to a calcium-deficient hydroxyapatite (CDHA), Ca9(HPO4)(PO4)5O H, whereas DCP did not react significantly; 2) the reaction was nearly finished within 32 h, during which both the reaction percentage and the compressive strength increased versus time, with a strong correlation between them; and 3) the calcium phosphate bone cement showed in general a structure of groups of interconnected large plates distributed among agglomerations of small crystal plates arranged in very dense packings.

  13. Pulsed electrodeposition for the synthesis of strontium-substituted calcium phosphate coatings with improved dissolution properties

    Energy Technology Data Exchange (ETDEWEB)

    Drevet, Richard, E-mail: richard.drevet@univ-reims.fr; Benhayoune, Hicham

    2013-10-15

    Strontium-substituted calcium phosphate coatings are synthesized by pulsed electrodeposition on titanium alloy (Ti6Al4V) substrates. Experimental conditions of the process are optimized in order to obtain a coating with a 5% atomic substitution of calcium by strontium which corresponds to the best observations on the osteoblast cells activity and on the osteoclast cells proliferation. The physical and chemical characterizations of the obtained coating are carried out by scanning electron microscopy associated to energy dispersive X-ray spectroscopy (EDXS) for X-ray microanalysis and the structural characterization of the coating is carried out by X-ray diffraction. The in vitro dissolution/precipitation properties of the coated substrates are investigated by immersion into Dulbecco's Modified Eagle Medium (DMEM) from 1 h to 14 days. The calcium, phosphorus and strontium concentrations variations in the biological liquid are assessed by Induced Coupled Plasma - Atomic Emission Spectroscopy for each immersion time. The results show that under specific experimental conditions, the electrodeposition process is suitable to synthesize strontium-substituted calcium phosphate coatings. Moreover, the addition of hydrogen peroxide (H{sub 2}O{sub 2}) into the electrolytic solution used in the process allows us to observe a control of the strontium release during the immersion of the prosthetic materials into DMEM. - Highlights: • Strontium-substituted calcium phosphate coatings are successfully electrodeposited. • The strontium is homogeneously distributed in the synthesized prosthetic coating. • This divalent cation modifies the calcium phosphate structure. • H{sub 2}O{sub 2} addition in the electrolyte allows to control the coating's stoichiometry. • This implies a control of the strontium release in the physiological environment.

  14. Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

    Science.gov (United States)

    Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

    2016-10-01

    Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

  15. Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

    Directory of Open Access Journals (Sweden)

    S. F. Mansour

    2015-11-01

    Full Text Available Abstract Hydroxyapatite (HAP and dicalcium phosphate dihydrate (brushite nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD, Fourier transformation infra-red spectroscopy (FTIR and thermo-gravimetric analysis (TGA. Scanning electron microscopy (SEM and transmission electron microscope (TEM were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

  16. Dynamic changes in calcium and phosphate plasma concentrations in the patients on peritoneal dialysis

    Directory of Open Access Journals (Sweden)

    Jovanović Nataša

    2006-01-01

    Full Text Available Background/Aim. The disturbances of active forms of vitamin D synthesis and disturbances in calcium and posphate metabolism develop early in chronic renal failure, when creatinine clearance is about 30 ml/min. Chronic hemodialysis and peritoneal dialysis only partially correct the biochemical environment of patients on chronic renal replacement therapy because of end-stage renal disease. These dialysis modalities can’t significantly affect the endocrine disturbances of chronic renal failure and they have minimal modulatory effect. The management of disturbed calcium (Ca and phosphate (P metabolism and the maintainance of Ca × P product below 4.4 mmol/l thanks to the use of dialysate solutions with the appropriate calcium concentration and the careful dosage of phosphate binders, calcium and active vitamin D metabolits, are extremely important for the prevention of renal osteodystrophy, secondary hyperparathyroidism as well as low-bone turnover disease. The aim of the study was to analyze the plasma levels of calcium, phosphate, albumin, alkaline phosphatase and parathormon (PTH in 58 patients who were treated with continuous ambulatory peritoneal dialysis (CAPD from March to August 2003. The use of phosphate binders and the substitution with active vitamin D metabolits were also analyzed. Methods. We examined 58 patients, 30 males and 28 female, mean-age 52 years (range, 26-78 years, affected by end-stage renal disease of the different leading cause. The average time on peritoneal dialysis program was 20 months (2-66 months. Most of the patients were treated by CAPD, while only few of them performed automatic, cyclic or intermittent peritoneal dialysis. Most of the patients used a dialysate with 1.75 mmol/l calcium concentration. Results. The study showed that our patients on chronic CAPD program during several months had normal calcemia, phosphatemia and the level of alkaline phosphatase, and that they had Ca × P product in the recommended

  17. Effect of Fluoride, Casein Phosphopeptide–Amorphous Calcium Phosphate and Casein Phosphopeptide–Amorphous Calcium Phosphate Fluoride on Enamel Surface Microhardness After Microabrasion: An In Vitro Study

    Directory of Open Access Journals (Sweden)

    Ghazaleh Ahmadi Zenouz

    2016-03-01

    Full Text Available Objectives: This study aimed to assess the effect of applying casein phosphopeptide–amorphous calcium phosphate (CPP-ACP paste, casein phosphopeptide–amorphous calcium phosphate fluoride (CPP-ACPF paste and sodium fluoride gel on surface microhardness of enamel after microabrasion.Materials and Methods: Thirty freshly extracted human premolars were selected. All samples were subjected to hardness indentations made with the Vickers hardness machine and the average value was recorded as the initial surface microhardness. The specimens were then randomly divided into three groups (n=10 of CPP-ACPF, fluoride and CPP-ACP. The teeth were micro-abraded with Opalustre. Microhardness test was performed to assess the post-abrasion hardness. Three remineralization modalities were performed on samples of each group. The enamel surface microhardness measurements were performed. To compare the difference between groups, the rehardening and softening values were defined. One-way ANOVA and Tukey’s post hoc test at a significance level of 5% were used for statistical analysis.Results: The mean microhardness value (MMV had a significant decrease after microabrasion from baseline. The MMV had a significant increase after remineralization in all groups. The MMV of CPP-ACPF group was significantly more than that of fluoride group (P=0.027. The rehardening value of fluoride group was significantly more than that of other groups (P<0.001.Conclusion: All the remineralizing agents were effective for rehardening the enamel after microabrasion. The CPP-ACP and CPP-ACPF pastes are effective, but to a lesser extent than neutral sodium fluoride gel in remineralizing enamel surface. Incorporation of fluoride to CPP-ACP formulation does not provide any additional remineralizing potential.Keywords: Casein phosphopeptide-amorphous calcium phosphate nanocomplex; Enamel Microabrasion; Hardness; Sodium Fluoride

  18. In vitro aging of a calcium phosphate cement.

    Science.gov (United States)

    Bohner, M; Merkle, H P; Lemaître, J

    2000-03-01

    Cement samples made of beta-tricalcium phoshate (beta-TCP), phosphoric acid (PA) and water mixtures were incubated in several aqueous solutions to determine their stability over time. The effects of the cement composition and the incubating temperature were investigated in more detail. The cement samples contained mostly dicalcium phosphate dihydrate (DCPD) and remnants of beta-TCP crystals. Depending on the initial cement composition, a certain amount of dicalcium phosphate (DCP) crystals were formed. The larger the initial PA concentration, the larger the DCP amount. After setting, the cement composition was stable for at least 16 days up to 60 degrees C. Above that temperature, the DCPD crystals decomposed into DCP crystals. The latter reaction provoked a decrease of the pH of the incubation solution, phenomenon expected for a cement sample containing an excess of PA. As the cement samples contained an excess of beta-TCP, it was postulated that beta-TCP crystals became so covered by DCP or DCPD crystals during setting that the setting reaction was stopped prematurely. The latter phenomenon gave a good explanation for the low pH values measured in the incubation solutions.

  19. Calcium Carbonate versus Sevelamer Hydrochloride as Phosphate Binders after Long-Term Disease Progression in 5/6 Nephrectomized Rats

    Directory of Open Access Journals (Sweden)

    Suvi Törmänen

    2014-01-01

    Full Text Available Our aim was to compare the effects of calcium carbonate and sevelamer-HCl treatments on calcium-phosphate metabolism and renal function in 5/6 nephrectomized (NX rats so that long-term disease progression preceded the treatment. After 15-week progression, calcium carbonate (3.0%, sevelamer-HCl (3.0%, or control diets (0.3% calcium were given for 9 weeks. Subtotal nephrectomy reduced creatinine clearance (−40%, plasma calcidiol (−25%, and calcitriol (−70% and increased phosphate (+37%, parathyroid hormone (PTH (11-fold, and fibroblast growth factor-23 (FGF-23 (4-fold. In NX rats, calcium carbonate diet increased plasma (+20% and urinary calcium (6-fold, reduced plasma phosphate (−50% and calcidiol (−30%, decreased creatinine clearance (−35% and FGF 23 (−85%, and suppressed PTH without influencing blood pH. In NX rats, sevelamer-HCl increased urinary calcium (4-fold and decreased creatinine clearance (−45%, PTH (−75%, blood pH (by 0.20 units, plasma calcidiol (−40%, and calcitriol (−65%. Plasma phosphate and FGF-23 were unchanged. In conclusion, when initiated after long-term progression of experimental renal insufficiency, calcium carbonate diet reduced plasma phosphate and FGF-23 while sevelamer-HCl did not. The former induced hypercalcemia, the latter induced acidosis, while both treatments reduced vitamin D metabolites and deteriorated renal function. Thus, delayed initiation influences the effects of these phosphate binders in remnant kidney rats.

  20. Development of a fully injectable calcium phosphate cement for orthopedic and dental applications

    Indian Academy of Sciences (India)

    Manoj Komath; H K Varma

    2003-06-01

    A study on the development of a fully injectable calcium phosphate cement for orthopedic and dental applications is presented. The paper describes its characteristic properties including results of bio- compatibility studies. A conventional two-component calcium phosphate cement formulation (having a powder part containing dry mixture of acidic and basic calcium phosphate particles and a liquid part containing phosphate solution) is modified with a biocompatible gelling agent, to induce flow properties and cohesion. The quantity of the gelling agent is optimized to get a viscous paste, which is smoothly injectable through an 18-gauge needle, with clinically relevant setting parameters. The new formulation has a setting time of 20 min and a compressive strength of 11 MPa. The X-ray diffraction, Fourier transform infrared spectrometry, and energy dispersive electron microprobe analyses showed the phase to be hydroxyapatite, the basic bone mineral. Scanning electron microscopy revealed a porous structure with particle sizes of a few micrometers. The cement did not show any appreciable dimensional or thermal change during setting. The injectability is estimated by extruding through needle and the cohesive property is assessed by water contact method. The cement passed the in vitro biocompatibility screening (cytotoxicity and haemolysis) tests.

  1. ATR-FTIR measurements of albumin and fibrinogen adsorption: Inert versus calcium phosphate ceramics.

    Science.gov (United States)

    Boix, Marcel; Eslava, Salvador; Costa Machado, Gil; Gosselin, Emmanuel; Ni, Na; Saiz, Eduardo; De Coninck, Joël

    2015-11-01

    Arthritis, bone fracture, bone tumors and other musculoskeletal diseases affect millions of people across the world. Nowadays, inert and bioactive ceramics are used as bone substitutes or for bone regeneration. Their bioactivity is very much dictated by the way proteins adsorb on their surface. In this work, we compared the adsorption of albumin and fibrinogen on inert and calcium phosphates ceramics (CaPs) using attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) to follow in situ protein adsorption on these materials. To this effect, we developed a sol-gel technique to control the surface chemistry of an ATR-FTIR detector. Hydroxyapatite adsorbed more albumin and β-tricalcium phosphate adsorbed more fibrinogen. Biphasic calcium phosphate presented the lowest adsorption among CaP for both proteins, illustrating the effect of surface heterogeneities. Inert ceramics adsorbed a lower amount of both proteins compared with bioactive ceramics. A significant change was observed in the conformation of the adsorbed protein versus the surface chemistry. Hydroxyapatite produced a larger loss of α-helix structure on albumin and biphasic calcium phosphate reduced β-sheet percentage on fibrinogen. Inert ceramics produced large α-helix loss on albumin and presented weak interaction with fibrinogen. Zirconia did not adsorb albumin and titanium dioxide promoted huge denaturalization of fibrinogen.

  2. Structural characterization of anion-calcium-humate complexes in phosphate-based fertilizers.

    Science.gov (United States)

    Baigorri, Roberto; Urrutia, Oscar; Erro, Javier; Mandado, Marcos; Pérez-Juste, Ignacio; Garcia-Mina, José María

    2013-07-01

    Fertilizers based on phosphate-metal-humate complexes are a new family of compounds that represents a more sustainable and bioavailable phosphorus source. The characterization of this type of complex by using solid (31)P NMR in several fertilizers, based on single superphosphate (SSP) and triple superphosphate (TSP) matrices, yielded surprising and unexpected trends in the intensity and fine structure of the (31)P NMR peaks. Computational chemistry methods allowed the characterization of phosphate-calcium-humate complexes in both SSP and TSP matrices, but also predicted the formation of a stable sulfate-calcium-humate complex in the SSP fertilizers, which has not been described previously. The stability of this complex has been confirmed by using ultrafiltration techniques. Preference towards the humic substance for the sulfate-metal phase in SSP allowed the explanation of the opposing trends that were observed in the experimental (31)P NMR spectra of SSP and TSP samples. Additionally, computational chemistry has provided an assignment of the (31)P NMR signals to different phosphate ligands as well as valuable information about the relative strength of the phosphate-calcium interactions within the crystals.

  3. Ectopic osteoid and bone formation by three calcium-phosphate ceramics in rats, rabbits and dogs.

    Directory of Open Access Journals (Sweden)

    Liao Wang

    Full Text Available Calcium phosphate ceramics with specific physicochemical properties have been shown to induce de novo bone formation upon ectopic implantation in a number of animal models. In this study we explored the influence of physicochemical properties as well as the animal species on material-induced ectopic bone formation. Three bioceramics were used for the study: phase-pure hydroxyapatite (HA sintered at 1200°C and two biphasic calcium phosphate (BCP ceramics, consisting of 60 wt.% HA and 40 wt.% TCP (β-Tricalcium phosphate, sintered at either 1100°C or 1200°C. 108 samples of each ceramic were intramuscularly implanted in dogs, rabbits, and rats for 6, 12, and 24 weeks respectively. Histological and histomorphometrical analyses illustrated that ectopic bone and/or osteoid tissue formation was most pronounced in BCP sintered at 1100°C and most limited in HA, independent of the animal model. Concerning the effect of animal species, ectopic bone formation reproducibly occurred in dogs, while in rabbits and rats, new tissue formation was mainly limited to osteoid. The results of this study confirmed that the incidence and the extent of material-induced bone formation are related to both the physicochemical properties of calcium phosphate ceramics and the animal model.

  4. Synthesis of some calcium phosphate crystals using the useful biomass for immobilization of microorganisms

    Science.gov (United States)

    Kohiruimaki, T.

    2011-10-01

    Three sources of biomass generated by primary industry were used as the raw material for the synthesis of calcium phosphate crystals. Phosphoric acid was extracted from burned rice chaff using a 30% nitric acid solution, while scallop shells and gypsum of plasterboard were used as calcium sources. The calcium phosphate crystals were synthesized by a method involving homogeneous precipitation, and the relationship between the composition and shape of the crystals and the pH at the time of the precipitation was investigated. Monetite crystals in a petal form with a diameter ranging from 0.1 to 2 μm were precipitated at pH 2.0, while granular apatite crystals with a mean diameter of 1 μm were precipitated at pH 6.0. We also investigated the ability of the synthesized calcium phosphate crystals to immobilize lactic acid bacteria for practical use in industrial bioreactor. It was determined that monetite crystals with a diameter of 2 μm had the highest ability to fix lactic acid bacteria. The population of lactic acid bacteria was estimated to exceed 1,300 bacteria per crystal surface of 50 μm2 suggesting that these crystals may be of practical use in industrial fermenters.

  5. Synthesis of some calcium phosphate crystals using the useful biomass for immobilization of microorganisms

    Energy Technology Data Exchange (ETDEWEB)

    Kohiruimaki, T, E-mail: kohi@hi-tech.ac.jp [Department of Technology, Hachinohe Institute of Technology, 88-1 Myo-oobiraki, Hachinohe-shi 031-8501 (Japan)

    2011-10-29

    Three sources of biomass generated by primary industry were used as the raw material for the synthesis of calcium phosphate crystals. Phosphoric acid was extracted from burned rice chaff using a 30% nitric acid solution, while scallop shells and gypsum of plasterboard were used as calcium sources. The calcium phosphate crystals were synthesized by a method involving homogeneous precipitation, and the relationship between the composition and shape of the crystals and the pH at the time of the precipitation was investigated. Monetite crystals in a petal form with a diameter ranging from 0.1 to 2 {mu}m were precipitated at pH 2.0, while granular apatite crystals with a mean diameter of 1 {mu}m were precipitated at pH 6.0. We also investigated the ability of the synthesized calcium phosphate crystals to immobilize lactic acid bacteria for practical use in industrial bioreactor. It was determined that monetite crystals with a diameter of 2 {mu}m had the highest ability to fix lactic acid bacteria. The population of lactic acid bacteria was estimated to exceed 1,300 bacteria per crystal surface of 50 {mu}m{sup 2} suggesting that these crystals may be of practical use in industrial fermenters.

  6. Magnesium substitution in the structure of orthopedic nanoparticles: A comparison between amorphous magnesium phosphates, calcium magnesium phosphates, and hydroxyapatites

    Energy Technology Data Exchange (ETDEWEB)

    Nabiyouni, Maryam, E-mail: maryam.nabiyouni@rockets.utoledo.edu [Department of Bioengineering, University of Toledo, Toledo, OH (United States); Ren, Yufu [Department of Mechanical, Industrial and Manufacturing Engineering, University of Toledo, Toledo, OH (United States); Bhaduri, Sarit B. [Department of Mechanical, Industrial and Manufacturing Engineering, University of Toledo, Toledo, OH (United States); Department of Surgery (Dentistry), University of Toledo, Toledo, OH (United States)

    2015-07-01

    As biocompatible materials, magnesium phosphates have received a lot of attention for orthopedic applications. During the last decade multiple studies have shown advantages for magnesium phosphate such as lack of cytotoxicity, biocompatibility, strong mechanical properties, and high biodegradability. The present study investigates the role of Mg{sup +2} and Ca{sup +2} ions in the structure of magnesium phosphate and calcium phosphate nanoparticles. To directly compare the effect of Mg{sup +2} and Ca{sup +2} ions on structure of nanoparticles and their biological behavior, three groups of nanoparticles including amorphous magnesium phosphates (AMPs) which release Mg{sup +2}, calcium magnesium phosphates (CMPs) which release Mg{sup +2} and Ca{sup +2}, and hydroxyapatites (HAs) which release Ca{sup +2} were studied. SEM, TEM, XRD, and FTIR were used to evaluate the morphology, crystallinity, and chemical properties of the particles. AMP particles were homogeneous nanospheres, whereas CMPs were combinations of heterogeneous nanorods and nanospheres, and HAs which contained heterogeneous nanosphere particles. Cell compatibility was monitored in all groups to determine the cytotoxicity effect of particles on studied MC3T3-E1 preosteoblasts. AMPs showed significantly higher attachment rate than the HAs after 1 day and both AMPs and CMPs showed significantly higher proliferation rate when compared to HAs after 7 days. Gene expression level of osteoblastic markers ALP, COL I, OCN, OPN, RUNX2 were monitored and they were normalized to GAPDH housekeeping gene. Beta actin expression level was monitored as the second housekeeping gene to confirm the accuracy of results. In general, AMPs and CMPs showed higher expression level of osteoblastic genes after 7 days which can further confirm the stimulating role of Mg{sup +}2 and Ca{sup +2} ions in increasing the proliferation rate, differentiation, and mineralization of MC3T3-E1 preosteoblasts. - Highlights: • Role of Mg{sup 2

  7. Investigation into the role of NaOH and calcium ions in the synthesis of calcium phosphate nanoshells

    Directory of Open Access Journals (Sweden)

    C. H. Yeo

    2012-03-01

    Full Text Available Calcium phosphate (CaP nanoshells were prepared using negatively charged liposomes (1,2-dioleoyl-sn-glycero-3-phosphate sodium salt (DOPA as a template by base titration synthesis at various concentrations of NaOH and calcium ions. The elemental composition, morphology, particle size, particle size distribution and zeta potential of the products were determined via various characterisation techniques, such as energy-dispersive X-ray spectrometry (EDX, transmission electron microscopy (TEM, dynamic light scattering (DLS, laser Doppler velocimetry (LDV and Fourier transform infrared spectroscopy (FTIR. The best results showed that stable spherical CaP nanoshells with a mean particle size of 197.5 ± 5.8 nm and a zeta potential of -34.5 ± 0.6 mV were successfully formed when 0.100 M sodium hydroxide (NaOH and 0.100 M calcium ions were used. Moreover, an optimal pH of 10.52 and a final Ca/P molar ratio of 0.97 were achieved under these conditions.

  8. Study of calcium phosphate (DCPD electrodeposition process on a Mg-3Al-1Zn magnesium alloy surface

    Directory of Open Access Journals (Sweden)

    Filip Pastorek

    2013-02-01

    Full Text Available Evaluation of calcium phosphating process realized on Mg-3Al-1Zn alloy surface after grinding was investigated by electrochemical tests supported by photodocumentation. The electrodeposition treatment was performed by electrochemical method in water solution of Ca(NO32.4H2O, (NH42HPO4 and H2O2. The formation of calcium phosphate was divided into several stages and described using light microscopy. The progress in corrosion protection of created calcium phosphate layer in 0.9% NaCl after particular electrodeposition steps was evaluated by electrochemical impedance spectroscopy. The results in the form of Nyquist plots were analyzed using equivalent circuits.

  9. On the Pressure-Induced Loss of Crystallinity in Zinc- and Calcium-Phosphates

    Energy Technology Data Exchange (ETDEWEB)

    Shakhvorostov, D.; Mosey, N; Munoz-Paniagua, D; Pereira, G; Song, Y; Kasrai, M; Norton, P; Müser, M

    2008-01-01

    A recently suggested mechanism for the stress memory of various metal phosphates is investigated experimentally. Based on first-principles simulations [N. J. Mosey et al., Science 307, 1612 (2005)], it had been argued that atoms with flexible coordination, such as zinc or heavy-metal cations, act as network-forming agents, undergoing irreversible pressure-induced changes in bonding that lead to increased connectivity between phosphate anions. In the present study, orthophosphates of zinc and calcium were exposed to high pressures on surfaces and in diamond anvil cells. An additional set of first-principles simulations was accomplished on ?-orthophosphate of zinc, which suggested that this material was already cross-linked before compression but that it nevertheless underwent a reversible coordination change under pressure in agreement with the experimental results presented here. Raman spectra indicate an irreversible, pressure-induced loss of long-range crystallinity. The pressures required to induce these changes are around 7 GPa for the zinc phosphates, while they are close to 21 GPa for the calcium phosphates. Hydrogenation of the metal phosphate lowers the threshold pressure by approximately 2-3 GPa in both cases. Moreover, ?-orthophosphate of zinc could be partially amorphisized under nonisotropic pressure on copper foils.

  10. An experimental approach to the study of the rheology behaviour of synthetic bone calcium phosphate cements

    Energy Technology Data Exchange (ETDEWEB)

    Friberg, J.; Fernandez, E.; Sarda, S.; Nilsson, M.; Ginebra, M.P.; Planell, J.A. [Universidad Politecnica de Catalunya, Barcelona (Spain). Dept. of Materials Science and Metallurgical Engineering; Martinez, S. [Barcelona Univ. (Spain). Mineralogia i Recursos Minerals

    2001-07-01

    Calcium phosphate cements were developed to fit surgical needs in biomedical fields such as odontology or traumatology. Nowadays, a broad field of new applications have been found for this kind of materials. Drug delivery systems, tissue-engineering scaffolds and osteoporotic bone filling applications are some of the new fields that are being benefited with these materials. Looking at both, commercial and new experimental calcium phosphate cements it is found that {alpha}-tricalcium phosphate is the main reactive powder responsible for the setting and the hardening of the cement. Thus, it is important to know how {alpha}-tricalcium phosphate affects injectability of these cements. The aim of this study was to investigate the rheological behaviour of {alpha}-tricalcium phosphate slurries in order to know how the cement injectability should be modified. Factors such as liquid to powder ratio, particle size of the main reactive powder and the addition of dispersants have been considered. The results showed that viscosity decreased when particle size of reactant was increased and when liquid to powder ratio was increased. It was also found that a minimum of viscosity exists at an optimum value of the weight percentage of dispersant. (orig.)

  11. The progress of early phase bone healing using porous granules produced from calcium phosphate cement

    Directory of Open Access Journals (Sweden)

    Jungbluth P

    2010-05-01

    Full Text Available Abstract Objective Bone grafting is a vital component in many surgical procedures to facilitate the repair of bone defects or fusions. Autologous bone has been the gold standard to date in spite of associated donor-site morbidity and the limited amount of available donor bone. The aim of this study was to investigate the progress of bone regeneration and material degradation of calcium phosphate granules (CPG produced from a calcium phosphate self-setting cement powder compared to the use of autologous bone grafting in the treatment of "critical size defects" on load-bearing long bones of minipigs. Methods A critical size defect in the tibial metaphysis of 16 mini-pigs was filled either with autologous cancellous graft or with micro- and macroporous carbonated, apatic calcium phosphate granules (CPG produced from a calcium phosphate self-setting cement powder. After 6 weeks, the specimens were assessed by X-ray and histological evaluation. The amount of new bone formation was analysed histomorphometrically. Results The semi-quantitative analysis of the radiological results showed a complete osseous bridging of the defect in three cases for the autograft group. In the same group five animals showed a beginning, but still incomplete bridging of the defect, whereas in the CPG group just two animals developed this. All other animals of the CPG group showed only a still discontinuous new bone formation. Altogether, radiologically a better osseous bridging was observed in the autograft group compared to the CPG group. Histomorphometrical analysis after six weeks of healing revealed that the area of new bone was significantly greater in the autograft group concerning the central area of the defect zone (p Conclusions Within the limits of the present study it could be demonstrated that autologous cancellous grafts lead to a significantly better bone regeneration compared to the application of calcium phosphate granules (CPG produced from a calcium

  12. Microanalyses of the hydroxyl-poly-calcium sodium phosphate coatings produced by ion beam assisted deposition

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Thin calcium phosphate coatings on titanium alloy substrates wereprepared by Ar+ ion beam assisted deposition (IBAD) from hydroxyl-poly-calciumsodium phosphate (HPPA) target. The coatings were analyzed by XRD, FTIR, XPS.These analyses revealed that the as-deposited films were amorphous or no apparentcrystallinity. No distinct absorption band of the hydroxyl group was observed in FTIRspectra of the coatings but new absorption bands were presented for CO3-2. Thecalcium to phosphorous ratio of these coatings in different IBAD conditions variedfrom 0.46 to 3.36.

  13. [Cognitive Function and Calcium. The relationship between inositol phosphates and brain function].

    Science.gov (United States)

    Nagata, Eiichiro

    2015-02-01

    Inositol phosphates are produced depending on the numbers of the phosphate group which is added to the inositol ring which is 6 membered ring derived from a component of a biological membrane. Inositol 1, 4, 5 trisphosphate (IP3) operates on IP3 receptor on the endoplasmic reticulum, and is related to a release of calcium in the cell. IP3 is associated with various brain functions and neurodegenerative disorders. Moreover, there are IP4, IP5, IP6 and IP7 such as inositol polyphosphates in mammals. Notably, inositol hexakisphoshate kinase (IP6) which phosphorylates IP6 to IP7 plays important roles in the pathophysiology of various neurodegenerative disorders.

  14. Phosphate removal using sludge from fuller's earth production.

    Science.gov (United States)

    Moon, Yong Hee; Kim, Jae Gon; Ahn, Joo Sung; Lee, Gyoo Ho; Moon, Hi-Soo

    2007-05-08

    This study assesses the phosphate removal capacity and mechanism of precipitation or adsorption from aqueous solutions in batch experiments by an industrial sludge containing gypsum (CaSO(4).2H(2)O) obtained as a by-product from a fuller's earth process. The potential capacity for phosphate removal was tested using various solution concentrations, pH values, reaction times, and amount of sludge. The maximum phosphate adsorption capacity calculated using the Langmuir equation was 2.0 g kg(-1). The pH for the maximum adsorption by the sludge was neutral to alkaline (pH 7-12). Over 99% of phosphate was removed from a phosphate solution of 30 mg L(-1) using 0.15 g of sludge in a 9-h reaction. Sulfate (SO(4)(2-)) concentration increased with increasing initial phosphate concentration, possibly because of dissolution of gypsum and adsorption of both sulfate and phosphate. At high phosphate concentration (>1000 mg L(-1)), relative constant concentration of Ca(2+) was not consistent with adsorption of the most important phosphate removal mechanism. Results suggest that precipitation of calcium phosphate is principally responsible for phosphate removal under its high concentration. Agglomerated precipitate in the reaction sludge was observed by SEM and identified as brushite (CaHPO(4).2H(2)O) by XRD, FT-IR, and DTA. Based on thermodynamic considerations, it is suggested that the brushite will readily transform to more stable phases, such as hydroxyapatite (Ca(5)(PO(4))(3).OH).

  15. Real-time monitoring of the setting reaction of brushite-forming cement using isothermal differential scanning calorimetry.

    Science.gov (United States)

    Hofmann, M P; Nazhat, S N; Gbureck, U; Barralet, J E

    2006-11-01

    The setting behavior of a brushite-forming cement (beta-tricalcium phosphate/mono calcium monophosphate) was investigated using an indentation technique (the Gillmore needles method) and isothermal differential scanning calorimetry (DSC). The two objectives of the study were to investigate whether DSC could be used to real-time monitor a fast-setting calcium phosphate cement (CPC) and to determine if it is possible to correlate DSC results directly with conventional setting-time measurements. Best-fit linear correlation analysis revealed that both the initial and final setting time (T(i) and T(f)) measured by indentation were strongly correlated to the maximum heat flow measured with DSC. It seems therefore possible to predict the setting times, usually achieved with user dependent indentation methods, of this specific fast setting CPC on the basis of objective DSC measurements. The drawbacks of DSC, however, are its overall complexity and expense and the fact that only exothermal reactions can be investigated in comparison to the Gillmore needles method, furthermore, it is not possible to monitor the complete reaction as the first 2 or 3 min are lost due to sample preparation and apparatus set up.

  16. Preparation and Properties of Nanoparticles of Calcium Phosphates With Various Ca/P Ratios.

    Science.gov (United States)

    Sun, Limin; Chow, Laurence C; Frukhtbeyn, Stanislav A; Bonevich, John E

    2010-01-01

    This study aimed at preparing and studying the properties of nanoparticles of calcium phosphate (nCaP) with Ca/P ratios ranging from 1.0 to 1.67 using a spray-drying technique. Micro-structural analyses suggested that the nCaPs with Ca/P ratios of 1.67 to 1.33 were nano-sized amorphous calcium phosphate (ACP) containing varying amounts of acid phosphate and carbonate. The nCaP with Ca/P ratio of 1 contained only nano-sized low crystalline dicalcium phosphate (DCP). BET measurements of the nCaPs showed specific surface areas of (12 ± 2 to 50 ± 1) m(2)/g, corresponding to estimated equivalent spherical diameters of (38 to 172) nm. However, dynamic light scattering measurements revealed much larger particles of (380 ± 49 to 768 ± 111) nm, owing to agglomeration of the smaller primary nano particles as revealed by Scanning Electron Microscopy (SEM). Thermodynamic solubility measurements showed that the nCaPs with Ca/P ratio of 1.33 - 1.67 all have similar solubility behavior. The materials were more soluble than the crystalline hydroxyapatite (HA) at pH greater than about 4.7, and more soluble than β-tricalcium phosphate (β-TCP), octacalcium phosphate (OCP) and DCP at pH above 5.5. Their solubility approached that of α-tricalcium phosphate (α-TCP) at about pH 7. These nCaPs, which cannot be readily prepared by other currently available methods for nanoparticle preparation, have potential biomedical applications.

  17. Calcium chloride and tricalcium phosphate effects on the pink color defect in cooked ground and intact turkey breast.

    Science.gov (United States)

    Sammel, L M; Claus, J R

    2007-12-01

    Calcium chloride (250, 500ppm) was examined for its ability to reduce the pink color defect induced by sodium nitrite (10ppm) and nicotinamide (1.0%) in cooked ground turkey in the presence and absence of sodium tripolyphosphate (0.25, 0.5%) and sodium citrate (0.5, 1.0%). The ability of tricalcium phosphate (0.1-0.5%) to reduce pink cooked color also was evaluated in ground turkey and both calcium chloride and tricalcium phosphate were tested for their effects on pink cooked color in whole breast muscle. The combination of calcium chloride and sodium tripolyphosphate, not calcium chloride alone, was necessary for a reduction in pink cooked color induced by nicotinamide. Subsequently, in the presence of phosphate, both calcium chloride and sodium citrate reduced pink cooked color and were most effective in combination. Tricalcium phosphate also was capable of reducing pink cooked color in ground turkey, however substituting tricalcium phosphate for sodium tripolyphosphate resulted in lower pH and cooking yields. Neither calcium chloride nor tricalcium phosphate was capable of reducing pink cooked color in whole turkey breast. Currently, a combination of sodium tripolyphosphate, calcium chloride, and sodium citrate represents the most suitable means for reducing or preventing the pink color defect in uncured ground turkey.

  18. Stabilization/solidification of mercury-contaminated waste ash using calcium sodium phosphate (CNP) and magnesium potassium phosphate (MKP) processes.

    Science.gov (United States)

    Cho, Jae Han; Eom, Yujin; Lee, Tai Gyu

    2014-08-15

    This study examined the stabilization and solidification (S/S) of mercury (Hg)-contaminated waste ash generated from an industrial waste incinerator using chemically bonded phosphate ceramic (CBPC) technology. A magnesium potassium phosphate (MKP; MgKPO4 · 6H2O) ceramic, fabricated from MgO and KH2PO4, and a calcium sodium phosphate (CNP; CaNaPO4) ceramic, fabricated from CaO and Na2HPO4, were used as solidification binders in the CBPC process, and Na2S or FeS was added to each solidification binder to stabilize the Hg-contaminated waste ash. The S/S processes were conducted under various operating conditions (based on the solidification binder and stabilization reagent, stabilization reagent dosage, and waste loading ratio), and the performance characteristics of the S/S sample under each operating condition were compared, including the Hg leaching value and compressive strength. The Hg leaching value of untreated Hg-contaminated waste ash was 231.3 μg/L, whereas the S/S samples treated using the MKP and CNP processes exhibited Hg leaching values below the universal treatment standard (UTS) limit (25 μg/L). Although the compressive strengths of the S/S samples decreased as the sulfide dosage and waste loading ratio were increased, most of the S/S samples fabricated by the MKP and CNP processes exhibited good mechanical properties.

  19. Effect of the temperature on the synthesis of dicalcium phosphate dihydrate

    Science.gov (United States)

    Dhiba, D.; Hakam, A.; El Khoukhi, H.; Albourine, A.; Nounah, A.

    2005-03-01

    The use of calcium phosphates as biomaterials was largely developed during the last decades. Among the phosphorous compounds solid minerals of biological interest, the dicalcium phosphate dihydrate, (DCPD or brushite) (CaHPO{4}, 2H{2}O), disserves a special attention. It can be prepared in different ways. The manufacture of inorganic phosphate, it is usually produced by the acidulation of limestone form of calcium with phosphoric acid. The synthesis of this phosphate depends on many operational parameters. This study was performed in order to verify the influence of temperature and the time on the chemical purity and the yield of precipitation. All the samples were characterized by X-ray diffraction, infrared spectrometry and chemical analysis.

  20. Brushite-collagen composites for bone regeneration.

    Science.gov (United States)

    Tamimi, Faleh; Kumarasami, Balamurugan; Doillon, Charles; Gbureck, Uwe; Le Nihouannen, Damien; Cabarcos, Enrique Lopez; Barralet, Jake E

    2008-09-01

    Brushite-based biomaterials are of special interest in bone regeneration due to their biocompatibility and biodegradability; on the other hand, collagen is a well-known osteoconductive biomaterial. In the present study a new brushite-collagen composite biomaterial is reported. This new biomaterial was prepared by combining citric acid/collagen type I solutions with a brushite cement powder. The obtained biomaterial was a cement paste, with improved handling properties. The effect of collagen on the setting reaction of brushite cement was studied, and was found to speed up the cement setting reaction. The cement paste set into a hard ceramic material within 18.5+/-2.1min and had compressive strength similar to that of spongeous bone (48.9+/-5.9MPa in dry conditions and 12.7+/-1.5MPa in humid conditions). The combination of collagen with citric acid revealed an interesting synergistic effect on the compressive strength of the composite material. Moreover, this new biomaterial had excellent cohesion properties (ninefold better than brushite cement), and high cellular adhesion capacity (threefold higher than brushite cement). The composite biomaterial described in this study combines good handling properties, compressive strength, cohesion and cell adhesion capacity, along with the osteoconductive and biodegradable properties inherent in brushite and in collagen-based biomaterials.

  1. Manufacturing of calcium phosphate scaffolds by pseudomorphic transformation of gypsum

    Energy Technology Data Exchange (ETDEWEB)

    Araujo Batista, H. de.; Batista Cardoso, M.; Sales Vasconcelos, A.; Vinicius Lia Fook, M.; Rodriguez Barbero, M. A.; Garcia Carrodeguas, R.

    2016-08-01

    Carbonated hydroxyapatite (CHAp) and β-tricalcium phosphate (β-TCP) have been employed for decades as constituents of scaffolds for bone regeneration because they chemically resemble bone mineral. In this study, the feasibility to manufacture CHAp/β-TCP scaffolds by pseudomorphic transformation of casted blocks of gypsum was investigated. The transformation was carried out by immersing the precursor gypsum block in 1 M (NH{sub 4}){sub 2}HPO{sub 4}/1.33 M NH{sub 4}OH solution with liquid/solid ratio of 10 mL/g and autoclaving at 120 degree centigrade and 203 kPa (2 atm) for 3 h at least. Neither shape nor dimensions significantly changed during transformation. The composition of scaffolds treated for 3 h was 70 wt.% CHAp and 30 wt.% β-TCP, and their compressive and diametral compressive strengths were 6.5 ± 0.7 and 5.3 ±0.7 MPa, respectively. By increasing the time of treatment to 6 h, the composition of the scaffold enriched in β-TCP (60 wt.% CHAp and 40 wt.% β-TCP) but its compressive and diametral compressive strengths were not significantly affected (6.7 ± 0.9 and 5.4 ± 0.6 MPa, respectively). On the basis of the results obtained, it was concluded that this route is a good approach to the manufacturing of biphasic (CHAp/β-TCP) scaffolds from previously shaped pieces of gypsum. (Author)

  2. Investigation on the biomimetic influence of biopolymers on calcium phosphate precipitation-Part 1: Alginate

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira de Lima, Daniel; Gomes Aimoli, Cassiano [Faculdade de Engenharia Quimica, Unicamp, CP6066 CEP13083-970, Campinas, SP (Brazil); Beppu, Marisa Masumi, E-mail: beppu@feq.unicamp.br [Faculdade de Engenharia Quimica, Unicamp, CP6066 CEP13083-970, Campinas, SP (Brazil)

    2009-05-05

    The understanding of how macromocules act in precipitation of inorganic phases is the key knowledge that is needed to establish the foundation to mimic nature and produce materials with high mechanical modulus besides outstanding optical and thermal properties. This study investigated how addition of small amounts of alginate (7-70 ppm), that presents many carboxylic groups, affects phase distribution and morphology of calcium phosphates, obtained through precipitation and further submitted to calcination and sintering. The results lead to the conclusion that alginate action is dynamic, where alginate molecules act as templates to nucleation, and most of the biopolymer remains in solution even when all calcium phosphate has precipitated. However, despite the effect on phase composition being mainly related to the system's kinetics, alginate does present thermodynamic interaction with the precipitates. It is probable that it acts by reducing the free energy of nucleation, as in heterogeneous nucleation processes.

  3. A brief review of calcium phosphate conversion coating on magnesium and its alloys

    Science.gov (United States)

    Zaludin, Mohd Amin Farhan; Jamal, Zul Azhar Zahid; Jamaludin, Shamsul Baharin; Derman, Mohd Nazree

    2016-07-01

    Recent developments have shown that magnesium is a promising candidate to be used as a biomaterial. Owing to its light weight, biocompatibility and compressive strength comparable with natural bones makes magnesium as an excellent choice for biomaterial. However, high reactivity and low corrosion resistance properties have restricted the application of magnesium as biomaterials. At the moment, several strategies have been developed to solve this problem. Surface modification of magnesium is one of the popular solutions to solve the problem. Among many techniques developed in the surface modification, conversion coating method is one of the simple and effective techniques. From various types of conversion coating, calcium phosphate-based conversion coating is the most suitable for biomedical fields. This paper reviews some studies on calcium phosphate coating on Mg and its alloys via chemical conversion method and discusses some factors determining the coating performance.

  4. Si-TCP synthesized from "Mg-free" reagents employed as calcium phosphate cement

    Directory of Open Access Journals (Sweden)

    Mariana Motisuke

    2012-08-01

    Full Text Available The influence of silicon doping on calcium phosphate cement were explored in this work. α-TCP and Si-α-TCP were prepared by solid state reaction employing "Mg-free" CaHPO4, CaCO3 and CaSiO3 as precursors. It was possible to obtain TCP powders with low contents of β phase as contaminant. Cement liquid phase was an aqueous solution containing 2.5 wt. (% of Na2HPO4 and 1.5 wt. (% of citric acid. The liquid-to-powder ratio was 0.6 mL.g-1. Chemical, physical and mechanical properties of the cement samples were determined by means of XRD, FTIR, XRF, compressive strength and SEM. The calcium phosphate cements obtained achieved satisfactory properties; however, Si-α-TCP presented a decrease on the rate of setting reaction.

  5. Effect of nanostructure on osteoinduction of porous biphasic calcium phosphate ceramics.

    Science.gov (United States)

    Li, Bo; Liao, Xiaoling; Zheng, Li; Zhu, Xiangdong; Wang, Zhe; Fan, Hongsong; Zhang, Xingdong

    2012-10-01

    In order to evaluate the effect of the nanostructure of calcium phosphate ceramics on osteoinductive potential, porous biphasic calcium phosphate (BCP) ceramics with a nano- or submicron structure were prepared via microwave sintering and compared to conventional BCP ceramics. The selective protein adsorption of bovine serum albumin and lysozyme (LSZ) and the osteogenic differentiation of human mesenchymal stem cells in vitro was investigated. Porous BCP nanoceramics showed higher ability to adsorb proteins, especially low molecular weight protein of LSZ, than conventional BCP ceramics, and the BCP nanoceramics promoted bone sialoprotein expression more than conventional BCP did. Further in vivo study to investigate ectopic bone formation and bone repair efficiency proved the highly osteoinductive potential of nanostructured BCP ceramics. The results suggest that nanostructured BCP ceramics have the potential to become a new generation of bioceramics for bone tissue engineering grafts.

  6. Influence of surface treatment of carbon fibers on electrochemical crystallization of calcium phosphate

    Institute of Scientific and Technical Information of China (English)

    TAO Ke; HUANG Su-ping; ZHOU Ke-chao

    2005-01-01

    Electrodeposition technique was used to coat calcium phosphate on carbon fiber which can be used to reinforce hydroxyapatite. The differences between fibers treated with and without nitric acid in electrodeposition were evaluated. The X-ray diffractometry results show that CaHPO4·2H2O is obtained as the kind of calcium phosphate coating on carbon fiber. The scanning electron microscopy photographs and deposit kinetic curve indicate that the influences of the functional group attained by nitric acid treatment, the crystal morphology and crystallization of the coating layers on the fiber with and without treatment rate are obviously different. The functional group, especially the acidic group, can act as nucleation centers of electrochemical crystallization.

  7. Calcium phosphate nanoparticles as versatile carrier for small and large molecules across cell membranes

    Energy Technology Data Exchange (ETDEWEB)

    Sokolova, Viktoriya; Rotan, Olga; Klesing, Jan [University of Duisburg-Essen, Inorganic Chemistry and Center for Nanointegration Duisburg-Essen (CeNIDE) (Germany); Nalbant, Perihan [University of Duisburg-Essen, Faculty of Biology, Institute of Molecular Cell Biology (Germany); Buer, Jan; Knuschke, Torben; Westendorf, Astrid M. [University Hospital Essen, University of Duisburg-Essen, Institute of Medical Microbiology (Germany); Epple, Matthias, E-mail: matthias.epple@uni-due.de [University of Duisburg-Essen, Inorganic Chemistry and Center for Nanointegration Duisburg-Essen (CeNIDE) (Germany)

    2012-06-15

    The successful transport of molecules across the cell membrane is a key point in biology and medicine. In most cases, molecules alone cannot penetrate the cell membrane, therefore an efficient carrier is needed. Calcium phosphate nanoparticles (diameter: 100-250 nm, depending on the functionalization) were loaded with fluorescent oligonucleotides, peptide, proteins, antibodies, polymers or porphyrins and characterized by dynamic light scattering, nanoparticle tracking analysis and scanning electron microscopy. Any excess of molecules was removed by ultracentrifugation, and the dissolved molecules at the same concentration were used as control. The uptake of such fluorescence-labeled nanoparticles into HeLa cells was monitored by fluorescence microscopy and confocal laser scanning microscopy. Calcium phosphate nanoparticles were able to transport all molecules across the cell membrane, whereas the dissolved molecules alone were taken up only to a very small extent or even not at all.

  8. Bioactive behavior of silicon substituted calcium phosphate based bioceramics for bone regeneration.

    Science.gov (United States)

    Khan, Ather Farooq; Saleem, Muhammad; Afzal, Adeel; Ali, Asghar; Khan, Afsar; Khan, Abdur Rahman

    2014-02-01

    Bone graft substitutes are widely used for bone regeneration and repair in defect sites resulting from aging, disease, trauma, or accident. With invariably increasing clinical demands, there is an urgent need to produce artificial materials, which are readily available and are capable of fast and guided skeletal repair. Calcium phosphate based bioactive ceramics are extensively utilized in bone regeneration and repair applications. Silicon is often utilized as a substituent or a dopant in these bioceramics, since it significantly enhances the ultimate properties of conventional biomaterials such as surface chemical structure, mechanical strength, bioactivity, biocompatibility, etc. This article presents an overview of the silicon substituted bioceramics, which have emerged as efficient bone replacement and bone regeneration materials. Thus, the role of silicon in enhancing the biological performance and bone forming capabilities of conventional calcium phosphate based bioceramics is identified and reviewed.

  9. The use of calcium phosphate-based biomaterials in implant dentistry.

    Science.gov (United States)

    Xie, Cheng; Lu, Hong; Li, Wei; Chen, Fa-Ming; Zhao, Yi-Min

    2012-03-01

    Since calcium phosphates (CaPs) were first proposed, a wide variety of formulations have been developed and continuously optimized, some of which (e.g. calcium phosphate cements, CPCs) have been successfully commercialized for clinical applications. These CaP-based biomaterials have been shown to be very attractive bone substitutes and efficient drug delivery vehicles across diverse biomedical applications. In this article, CaP biomaterials, principally CPCs, are addressed as alternatives/complements to autogenous bone for grafting in implant dentistry and as coating materials for enhancing the osteoinductivity of titanium implants, highlighting their performance benefits simultaneously as carriers for growth factors and as scaffolds for cell proliferation, differentiation and penetration. Different strategies for employing CaP biomaterials in dental implantology aim to ultimately reach the same goal, namely to enhance the osseointegration process for dental implants in the context of immediate loading and to augment the formation of surrounding bone to guarantee long-term success.

  10. Early resorption of an artificial bone graft made of calcium phosphate for cranioplasty: case report

    Directory of Open Access Journals (Sweden)

    Monaco BA

    2013-11-01

    Full Text Available Bernardo Assumpção de Monaco, Erich Talamoni Fonoff, Manoel Jacobsen TeixeiraDivision of Functional Neurosurgery, Department of Neurology, Hospital das Clinicas, University of São Paulo Medical School, São Paulo, BrazilAbstract: The treatment of uncomplicated osteoma consists of an en bloc resection, or curettage, of the tumor, followed by cranioplasty. Here, we present a case report of a patient treated for a parietal osteoma, followed by a calcium phosphate cranioplasty, with early resorption after 3 months, which was presented by a sinking flap above the resection area. This case suggests that synthetic cranioplasty should be preferred, even in small skull-gap areas.Keywords: cranioplasty, bone cement, osteoma, calcium phosphate, resorption

  11. Studies on the mechanisms underlying the transfer of calcium and phosphate from bone to blood

    Energy Technology Data Exchange (ETDEWEB)

    Brommage, Robert J. Jr.

    1978-01-01

    The skeleton is recognized as a crucial organ in the minute-to-minute regulation of the blood levels of calcium and phosphate. The fluxes of calcium and phosphate to and from bone greatly exceed the entry and exit of these ions occurring in the intestine and kidneys. Parathyroid hormone, calcitonin, and 1,25-dihydroxyvitamin D/sub 3/ (1,25-(OH)/sub 2/D/sub 3/ are known to influence the transfer of calcium and phosphate from bone to blood. Three mechanisms have been proposed to explain the hormonal control of the calcium and phosphate effluxes from bone. The concept of a bone membrane maintaining a distinct bone extracellular fluid composition has led to the pump and pH gradient theories. An alternate solubilizer theory proposes that bone cells secrete a substance which increases the solubility of the bone mineral. The bone membrane concept was originally proposed to explain the presence of the apparent anomalously high concentrations of potassium in the bone extracellular fluid. However, the available evidence does not allow an unambiguous decision concerning the presence of a bone membrane. Calvarial lactate production was unaltered by 1,25-(OH)/sub 2/D/sub 3/ treatment and consequently 1,25-(OH)/sub 2/D/sub 3/ does not appear to promote the mobilization of bone mineral through a lactate-mediated pH gradient mechanism. 1,25-(OH)/sub 2/D/sub 3/ did increase the solubility of non-vital bone, clearly demonstrating that the solubilizer mechanism is at least partially responsible for the mobilization of bone mineral and the regulation of blood levels of calcium and phosphate. Vitamin D-deficient female rats fed a 0.2% calcium, 0.4% phosphorous diet and supplemented with daily injections of 0.75 pmole of 1,25-(OH)/sub 2/D/sub 3/ were shown to be capable of bearing young. When the injections of 1,25-(OH)/sub 2/D/sub 3/ were terminated at delivery, the dams and pups showed signs of vitamin D deficiency approximately one week later.

  12. Calcium salts of keto-amino acids, a phosphate binder alternative for patients on CAPD.

    Science.gov (United States)

    Macia, M; Coronel, F; Navarro, J F; Gallego, E; Herrero, J A; Méndez, M L; Chahin, J; García, J

    1997-09-01

    Control of hyperphosphoremia is crucial to the prevention of secondary hyperparathyroidism. Calcium salts of keto-amino acids (KAA) were employed as phosphate binders in hemodialysis patients. We wanted to assess the efficacy of these substances as quelating agents in patients under continuous ambulatory peritoneal dialysis (CAPD). Also, as an amino acid supplement, we determined their possible effect on some parameters related to nutritional status. We studied 13 patients (7 M; 6 F) with a mean age of 45.2 +/- 17 years and a mean time on CAPD of 18.4 +/- 11.4 months. None had severe secondary hyperparathyroidism and/or clinically relevant aluminium intoxication. They were not receiving calcitriol and none were using low-calcium peritoneal dialysis fluids. All were under aluminum hydroxide (AlOH3) treatment and 8 patients also received calcium carbonate. These quelating agents were withdrawn and after 21 days (wash-out period) KAA were initiated. We analyzed serum levels of bone metabolism parameters (calcium, phosphate, osteocalcin [OC], intact parathyroid hormone [iPTH], alkaline phosphatase [AP]) and nutritional parameters (total protein, albumin, pre-albumin, transferrin) in four periods: (A) during AlOH3; (B) immediately after the washout period; (C) after 1.5 months; and (D) after 3 months of KAA therapy. In 5 patients serum aluminum level was also measured in periods (A) and (D). The serum phosphate level at period (B) was significantly higher than in other periods. After 3 months of treatment phosphate levels decreased significantly (A = 1.77 +/- 0.3 mmol/l vs D = 1.48 +/- 0.2; p < 0.05). Serum calcium levels increased, while iPTH and OC decreased (p = ns). AP remained stable during the study. All nutritional parameters increased at the end of the study (p = ns). Calcium salts of keto-amino acids showed to be an effective alternative to aluminum-containing phosphate binders. They were well tolerated, without relevant side-effects. These compounds could also

  13. Calcium phosphate cement as an alternative for formocresol in primary teeth pulpotomies

    OpenAIRE

    Bijimole Jose; Ratnakumari, N; Mira Mohanty; Varma, H. K.; Manoj Komath

    2013-01-01

    Background: Formocresol remains to be the preferred medicament in pulpotomy, despite the concerns regarding tissue devitalization and systemic toxicity. Several materials were used as alternatives, but none proved significantly advantageous. Of recent, calcium phosphate cement (CPC) has been projected as an ideal pulpotomy material considering its tissue compatibility and dentinogenic properties. This study explores the suitability of a CPC formulation for pulpotomy, in comparison with formoc...

  14. The effect of calcium phosphate nanoparticles on hormone production and apoptosis in human granulosa cells

    Directory of Open Access Journals (Sweden)

    Gao Li

    2010-04-01

    Full Text Available Abstract Objectives Although many nanomaterials are being used in academia, industry and daily life, there is little understanding about the effects of nanoparticles on the reproductive health of vertebral animals, including human beings. An experimental study was therefore performed here to explore the effect of calcium phosphate nanoparticles on both steroid hormone production and apoptosis in human ovarian granulosa cells. Methods Calcium phosphate nanoparticles uptaking was evaluated by transmission electron microscopy (TEM. The cell cycle was assessed with propidium iodide-stained cells (distribution of cells in G0/G1, S, and G2/M phases by flow cytometry. The pattern of cell death (necrosis and apoptosis was analyzed by flow cytometry with annexin V-FITC/PI staining. The expression of mRNAs encoding P450scc, P450arom and StAR were determined by RT-PCR. Progesterone and estradiol levels were measured by radioimmunoassay. Results TEM results confirmed that calcium phosphate nanoparticles could enter into granulosa cells, and distributed in the membranate compartments, including lysosome and mitochondria and intracellular vesicles. The increased percentage of cells in S phase when cultured with nanoparticles indicated that there was an arrest at the checkpoint from phase S-to-G2/M (from 6.28 +/- 1.55% to 11.18 +/- 1.73%, p Conclusion Calcium phosphate nanoparticles interfered with cell cycle of cultured human ovarian granulosa cells thus increasing cell apoptosis. This pilot study suggested that effects of nanoparticles on ovarian function should be extensively investigated.

  15. Effect of different calcium phosphate scaffold ratios on odontogenic differentiation of human dental pulp cells

    Energy Technology Data Exchange (ETDEWEB)

    AbdulQader, Sarah Talib [School of Dental Sciences, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan (Malaysia); Department of Pedodontic and Preventive Dentistry, College of Dentistry, University of Baghdad, Baghdad (Iraq); Kannan, Thirumulu Ponnuraj, E-mail: kannan@usm.my [School of Dental Sciences, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan (Malaysia); Human Genome Centre, School of Medical Sciences, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan (Malaysia); Rahman, Ismail Ab [School of Dental Sciences, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan (Malaysia); Ismail, Hanafi [School of Materials and Minerals Resource Engineering, Universiti Sains Malaysia, 14300 Penang (Malaysia); Mahmood, Zuliani [School of Dental Sciences, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan (Malaysia)

    2015-04-01

    Calcium phosphate (CaP) scaffolds have been widely and successfully used with osteoblast cells for bone tissue regeneration. However, it is necessary to investigate the effects of these scaffolds on odontoblast cells' proliferation and differentiation for dentin tissue regeneration. In this study, three different hydroxyapatite (HA) to beta tricalcium phosphate (β-TCP) ratios of biphasic calcium phosphate (BCP) scaffolds, BCP20, BCP50, and BCP80, with a mean pore size of 300 μm and 65% porosity were prepared from phosphoric acid (H{sub 2}PO{sub 4}) and calcium carbonate (CaCO{sub 3}) sintered at 1000 °C for 2 h. The extracts of these scaffolds were assessed with regard to cell viability and differentiation of odontoblasts. The high alkalinity, more calcium, and phosphate ions released that were exhibited by BCP20 decreased the viability of human dental pulp cells (HDPCs) as compared to BCP50 and BCP80. However, the cells cultured with BCP20 extract expressed high alkaline phosphatase activity and high expression level of bone sialoprotein (BSP), dental matrix protein-1 (DMP-1), and dentin sialophosphoprotein (DSPP) genes as compared to that cultured with BCP50 and BCP80 extracts. The results highlighted the effect of different scaffold ratios on the cell microenvironment and demonstrated that BCP20 scaffold can support HDPC differentiation for dentin tissue regeneration. - Highlights: • BCPs of different HA/β-TCP ratios influence cell microenvironment. • BCP20 decreases cell viability of HDPCs as compared to BCP50 and BCP80. • HDPCs cultured with BCP20 express highest ALP activity. • HDPCs cultured with BCP20 up-regulate BSP, DMP-1 and DSPP gene expressions. • BCP20 can support HDPC differentiation for dentin tissue regeneration.

  16. Calcium phosphate thin films enhance the response of human mesenchymal stem cells to nanostructured titanium surfaces

    Directory of Open Access Journals (Sweden)

    Mura M McCafferty

    2014-05-01

    Full Text Available The development of biomaterial surfaces possessing the topographical cues that can promote mesenchymal stem cell recruitment and, in particular, those capable of subsequently directing osteogenic differentiation is of increasing importance for the advancement of tissue engineering. While it is accepted that it is the interaction with specific nanoscale topography that induces mesenchymal stem cell differentiation, the potential for an attendant bioactive chemistry working in tandem with such nanoscale features to enhance this effect has not been considered to any great extent. This article presents a study of mesenchymal stem cell response to conformal bioactive calcium phosphate thin films sputter deposited onto a polycrystalline titanium nanostructured surface with proven capability to directly induce osteogenic differentiation in human bone marrow–derived mesenchymal stem cells. The sputter deposited surfaces supported high levels of human bone marrow–derived mesenchymal stem cell adherence and proliferation, as determined by DNA quantification. Furthermore, they were also found to be capable of directly promoting significant levels of osteogenic differentiation. Specifically, alkaline phosphatase activity, gene expression and immunocytochemical localisation of key osteogenic markers revealed that the nanostructured titanium surfaces and the bioactive calcium phosphate coatings could direct the differentiation towards an osteogenic lineage. Moreover, the addition of the calcium phosphate chemistry to the topographical profile of the titanium was found to induce increased human bone marrow–derived mesenchymal stem cell differentiation compared to that observed for either the titanium or calcium phosphate coating without an underlying nanostructure. Hence, the results presented here highlight that a clear benefit can be achieved from a surface engineering strategy that combines a defined surface topography with an attendant, conformal

  17. The In-situ Reinforcement of Calcium Phosphate Cement and Its Micro-structural Analysis

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Carbon nanotubes ( CNTs ) and polyacrylic acid were employed to modify the setting process and hydration products of β- TCP/ TTCP calcium phosphate cement. The micro-structure of hydration product and the fashion of how additives and hydration particles interconnected were investigated. With the modification effect of CNTs, the setting particles and CNTs got winded and interconnected and thus made the composite more compact and denser.

  18. Evaluation of implant calcium-phosphate materials depending on their mineral content

    Directory of Open Access Journals (Sweden)

    I. A. Talashova

    2012-01-01

    Full Text Available Biocompatibility of original implant calcium-phosphate materials was evaluated in the experiment on animals. The methods of radiological electron-probe microanalysis (REMA and light and scan electron microscopy (SEM were used. Studied materials had the properties of biodegradation, osteoinduction and osteoconduction at different extent. The materials with the composite maximally close to the the bone tissue had the greatest grade of biocompatibility.

  19. Structural changes to resorbable calcium phosphate bioceramic aged in vitro

    OpenAIRE

    Mehrban, Nazia; Bowen, James; Vorndran, Elke; Gbureck, Uwe; Liam M Grover

    2013-01-01

    This work investigates the effect of mammalian cell culture conditions on 3D printed calcium phosphate scaffolds. The purpose of the studies presented was to characterise the changes in scaffold properties in physiologically relevant conditions. Differences in crystal morphologies were observed between foetal bovine serum-supplemented media and their unsupplemented analogues, but not for supplemented media containing tenocytes. Scaffold porosity was found to increase for all conditions studie...

  20. Calcium gluconate in phosphate buffered saline increases gene delivery with adenovirus type 5.

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    Marko T Ahonen

    Full Text Available BACKGROUND: Adenoviruses are attractive vectors for gene therapy because of their stability in vivo and the possibility of production at high titers. Despite exciting preclinical data with various approaches, there are only a few examples of clear efficacy in clinical trials. Effective gene delivery to target cells remains the key variable determining efficacy and thus enhanced transduction methods are important. METHODS/RESULTS: We found that heated serum could enhance adenovirus 5 mediated gene delivery up to twentyfold. A new protein-level interaction was found between fiber knob and serum transthyretin, but this was not responsible for the observed effect. Instead, we found that heating caused the calcium and phosphate present in the serum mix to precipitate, and this was responsible for enhanced gene delivery. This finding could have relevance for designing preclinical experiments with adenoviruses, since calcium and phosphate are present in many solutions. To translate this into an approach potentially testable in patients, we used calcium gluconate in phosphate buffered saline, both of which are clinically approved, to increase adenoviral gene transfer up to 300-fold in vitro. Gene transfer was increased with or without heating and in a manner independent from the coxsackie-adenovirus receptor. In vivo, in mouse studies, gene delivery was increased 2-, 110-, 12- and 13-fold to tumors, lungs, heart and liver and did not result in increased pro-inflammatory cytokine induction. Antitumor efficacy of a replication competent virus was also increased significantly. CONCLUSION: In summary, adenoviral gene transfer and antitumor efficacy can be enhanced by calcium gluconate in phosphate buffered saline.

  1. Calcium Gluconate in Phosphate Buffered Saline Increases Gene Delivery with Adenovirus Type 5

    Science.gov (United States)

    Ahonen, Marko T.; Diaconu, Iulia; Pesonen, Sari; Kanerva, Anna; Baumann, Marc; Parviainen, Suvi T.; Spiller, Brad

    2010-01-01

    Background Adenoviruses are attractive vectors for gene therapy because of their stability in vivo and the possibility of production at high titers. Despite exciting preclinical data with various approaches, there are only a few examples of clear efficacy in clinical trials. Effective gene delivery to target cells remains the key variable determining efficacy and thus enhanced transduction methods are important. Methods/Results We found that heated serum could enhance adenovirus 5 mediated gene delivery up to twentyfold. A new protein-level interaction was found between fiber knob and serum transthyretin, but this was not responsible for the observed effect. Instead, we found that heating caused the calcium and phosphate present in the serum mix to precipitate, and this was responsible for enhanced gene delivery. This finding could have relevance for designing preclinical experiments with adenoviruses, since calcium and phosphate are present in many solutions. To translate this into an approach potentially testable in patients, we used calcium gluconate in phosphate buffered saline, both of which are clinically approved, to increase adenoviral gene transfer up to 300-fold in vitro. Gene transfer was increased with or without heating and in a manner independent from the coxsackie-adenovirus receptor. In vivo, in mouse studies, gene delivery was increased 2-, 110-, 12- and 13-fold to tumors, lungs, heart and liver and did not result in increased pro-inflammatory cytokine induction. Antitumor efficacy of a replication competent virus was also increased significantly. Conclusion In summary, adenoviral gene transfer and antitumor efficacy can be enhanced by calcium gluconate in phosphate buffered saline. PMID:20927353

  2. Polyfunctional bioceramics based on calcium phosphate and M-type hexagonal ferrite for medical applications

    Science.gov (United States)

    Tkachenko, M. V.; Ol'khovik, L. P.; Kamzin, A. S.; Keshri, S.

    2014-01-01

    Magnetic biologically active ceramics based on calcium phosphate with a content of M-type hexagonal ferrite (HF) particles varying from 10 to 50 wt % has been synthesized and characterized. It has been found that the ceramics synthesized consists of a biocompatible carbonated hydroxyapatite (CHA) with the matrix containing M-type HF particles, leading to the magnetic characteristics of the ceramics synthesized being significantly higher than those of iron-oxide-modified bioglass ceramics used in medicine.

  3. Controlled formation of calcium-phosphate-based hybrid mesocrystals by organic-inorganic co-assembly.

    Science.gov (United States)

    Zhai, Halei; Chu, Xiaobin; Li, Li; Xu, Xurong; Tang, Ruikang

    2010-11-01

    An understanding of controlled formation of biomimetic mesocrystals is of great importance in materials chemistry and engineering. Here we report that organic-inorganic hybrid plates and even mesocrystals can be conveniently synthesized using a one-pot reaction in a mixed system of protein (bovine serum albumin (BSA)), surfactant (sodium bis(2-ethylhexyl) sulfosuccinate (AOT)) and supersaturated calcium phosphate solution. The morphologies of calcium-phosphate-based products are analogous to the general inorganic crystals but they have abnormal and interesting substructures. The hybrids are constructed by the alternate stacking of organic layer (thickness of 1.31 nm) and well-crystallized inorganic mineral layer (thickness of 2.13 nm) at the nanoscale. Their morphologies (spindle, rhomboid and round) and sizes (200 nm-2 μm) can be tuned gradually by changing BSA, AOT and calcium phosphate concentrations. This modulation effect can be explained by a competition between the anisotropic and isotropic assembly of the ultrathin plate-like units. The anisotropic assembly confers mesocrystal characteristics on the hybrids while the round ones are the results of isotropic assembly. However, the basic lamellar organic-inorganic substructure remains unchanged during the hybrid formation, which is a key factor to ensure the self-assembly from molecule to micrometre scale. A morphological ternary diagram of BSA-AOT-calcium phosphate is used to describe this controlled formation process, providing a feasible strategy to prepare the required materials. This study highlights the cooperative effect of macromolecule (frame structure), small biomolecule (binding sites) and mineral phase (main component) on the generation and regulation of biomimetic hybrid mesocrystals.

  4. Role of 20-kDa amelogenin (P148) phosphorylation in calcium phosphate formation in vitro.

    Science.gov (United States)

    Kwak, Seo-Young; Wiedemann-Bidlack, Felicitas B; Beniash, Elia; Yamakoshi, Yasuo; Simmer, James P; Litman, Amy; Margolis, Henry C

    2009-07-10

    The potential role of amelogenin phosphorylation in enamel formation is elucidated through in vitro mineralization studies. Studies focused on the native 20-kDa porcine amelogenin proteolytic cleavage product P148 that is prominent in developing enamel. Experimental conditions supported spontaneous calcium phosphate precipitation with the initial formation of amorphous calcium phosphate (ACP). In the absence of protein, ACP was found to undergo relatively rapid transformation to randomly oriented plate-like apatitic crystals. In the presence of non-phosphorylated recombinant full-length amelogenin, rP172, a longer induction period was observed during which relatively small ACP nanoparticles were transiently stabilized. In the presence of rP172, these nanoparticles were found to align to form linear needle-like particles that subsequently transformed and organized into parallel arrays of apatitic needle-like crystals. In sharp contrast to these findings, P148, with a single phosphate group on serine 16, was found to inhibit calcium phosphate precipitation and stabilize ACP formation for more than 1 day. Additional studies using non-phosphorylated recombinant (rP147) and partially dephosphorylated forms of P148 (dephoso-P148) showed that the single phosphate group in P148 was responsible for the profound effect on mineral formation in vitro. The present study has provided, for the first time, evidence suggesting that the native proteolytic cleavage product P148 may have an important functional role in regulating mineralization during enamel formation by preventing unwanted mineral formation within the enamel matrix during the secretory stage of amelogenesis. Results obtained have also provided new insights into the functional role of the highly conserved hydrophilic C terminus found in full-length amelogenin.

  5. External bone remodeling after injectable calcium-phosphate cement in benign bone tumor: two cases in the hand.

    Science.gov (United States)

    Ichihara, S; Vaiss, L; Acciaro, A L; Facca, S; Liverneaux, P

    2015-12-01

    Bone remodeling commonly occurred after fracture and curettage benign bone tumor. A lot of previous articles reported "internal" trabecular bone remodeling. There were no previous clinical reports about "external" cortical bone remodeling. We present here 2 clinical cases of "external" bone remodeling after injectable calcium-phosphate in benign bone tumor in the hand. In two cases of benign bone tumor, we performed complete removal of the tumor and immediate filling of the metacarpal bone with injectable calcium-phosphate cement Arexbone(®) from the mechanical viewpoint. With respect to the shape of the calcium-phosphate, by using an injection-type, calcium-phosphate is adhered uniformly to the bone cortex by injecting, remodeling has been promoted. After 5 and 8years, both cases were no recurrences, and the shape of the metacarpal looked close to the contralateral side. These findings supposed to be concerned with potential self-healing and self-protection mechanism in human body.

  6. Kinetics of phosphate absorption in lactating dairy cows after enteral administration of sodium phosphate or calcium phosphate salts.

    Science.gov (United States)

    Grünberg, Walter; Dobbelaar, Paul; Breves, Gerhard

    2013-09-28

    Hypophosphataemia is frequently encountered in dairy cows during early lactation. Although supplementation of P is generally recommended, controversy exists over the suitability of oral P supplementation in animals with decreased or absent rumen motility. Since the effects of transruminal P absorption and the reticular groove reflex on the absorption kinetics of P are not well understood, it is unclear in how far treatment efficacy of oral P supplementation is affected by decreased rumen motility. Phosphate absorption was studied in six phosphate-depleted dairy cows fitted with rumen cannulas and treated with test solutions containing either NaH2PO4 or CaHPO4 with acetaminophen. Each animal was treated orally, intraruminally and intra-abomasally in randomised order. Absorption kinetics of P were studied and compared with the absorption kinetics of acetaminophen, a marker substance only absorbed from the small intestine. Intra-abomasal treatment with NaH2PO4 resulted in the most rapid and highest peaks in plasma inorganic P (Pi) concentration. Oral and intraruminal administration of NaH2PO4 resulted in similar increases in plasma Pi concentration from 4 to 7 h in both groups. Treatment with NaH2PO4 caused more pronounced peaks in plasma Pi concentration compared with CaHPO4. Neither transruminal P absorption nor the reticular groove reflex affected P absorption kinetics as determined by comparing plasma concentration–time curves of P and acetaminophen after administration of 1M-phosphate salt solutions. It is concluded that oral treatment with NaH2PO4 but not CaHPO4 is effective in supplementing P in hypophosphataemic cows with adequate rumen motility. Decreased rumen motility is likely to hamper the efficacy of oral phosphate treatment.

  7. 3D printing of composite calcium phosphate and collagen scaffolds for bone regeneration.

    Science.gov (United States)

    Inzana, Jason A; Olvera, Diana; Fuller, Seth M; Kelly, James P; Graeve, Olivia A; Schwarz, Edward M; Kates, Stephen L; Awad, Hani A

    2014-04-01

    Low temperature 3D printing of calcium phosphate scaffolds holds great promise for fabricating synthetic bone graft substitutes with enhanced performance over traditional techniques. Many design parameters, such as the binder solution properties, have yet to be optimized to ensure maximal biocompatibility and osteoconductivity with sufficient mechanical properties. This study tailored the phosphoric acid-based binder solution concentration to 8.75 wt% to maximize cytocompatibility and mechanical strength, with a supplementation of Tween 80 to improve printing. To further enhance the formulation, collagen was dissolved into the binder solution to fabricate collagen-calcium phosphate composites. Reducing the viscosity and surface tension through a physiologic heat treatment and Tween 80, respectively, enabled reliable thermal inkjet printing of the collagen solutions. Supplementing the binder solution with 1-2 wt% collagen significantly improved maximum flexural strength and cell viability. To assess the bone healing performance, we implanted 3D printed scaffolds into a critically sized murine femoral defect for 9 weeks. The implants were confirmed to be osteoconductive, with new bone growth incorporating the degrading scaffold materials. In conclusion, this study demonstrates optimization of material parameters for 3D printed calcium phosphate scaffolds and enhancement of material properties by volumetric collagen incorporation via inkjet printing.

  8. Physicochemical and Microstructural Characterization of Injectable Load-Bearing Calcium Phosphate Scaffold

    Directory of Open Access Journals (Sweden)

    Mazen Alshaaer

    2013-01-01

    Full Text Available Injectable load-bearing calcium phosphate scaffolds are synthesized using rod-like mannitol grains as porogen. These degradable injectable strong porous scaffolds, prepared by calcium phosphate cement, could represent a valid solution to achieve adequate porosity requirements while providing adequate support in load-bearing applications. The proposed process for preparing porous injectable scaffolds is as quick and versatile as conventional technologies. Using this method, porous CDHA-based calcium phosphate scaffolds with macropores sizes ranging from 70 to 300 μm, micropores ranging from 5 to 30 μm, and 30% open macroporosity were prepared. The setting time of the prepared scaffolds was 15 minutes. Also their compressive strength and e-modulus, 4.9 MPa and 400 MPa, respectively, were comparable with those of the cancellous bone. Finally, the bioactivity of the scaffolds was confirmed by cell growth with cytoplasmic extensions in the scaffolds in culture, demonstrating that the scaffold has a potential for MSC seeding and growth architecture. This combination of an interconnected macroporous structure with pore size suitable for the promotion of cell seeding and proliferation, plus adequate mechanical features, represents a porous scaffold which is a promising candidate for bone tissue engineering.

  9. The effect of porosity on drug release kinetics from vancomycin microsphere/calcium phosphate cement composites.

    Science.gov (United States)

    Schnieders, Julia; Gbureck, Uwe; Vorndran, Elke; Schossig, Michael; Kissel, Thomas

    2011-11-01

    The influence of porosity on release profiles of antibiotics from calcium phosphate composites was investigated to optimize the duration of treatment. We hypothesized, that by the encapsulation of vancomycin-HCl into biodegradable microspheres prior admixing to calcium phosphate bone cement, the influence of porosity of the cement matrix on vancomycin release could be reduced. Encapsulation of vancomycin into a biodegradable poly(lactic co-glycolic acid) copolymer (PLGA) was performed by spray drying; drug-loaded microparticles were added to calcium phosphate cement (CPC) at different powder to liquid ratios (P/L), resulting in different porosities of the cement composites. The effect of differences in P/L ratio on drug release kinetics was compared for both the direct addition of vancomycin-HCl to the cement liquid and for cement composites modified with vancomycin-HCl-loaded microspheres. Scanning electron microscopy (SEM) was used to visualize surface and cross section morphology of the different composites. Brunauer, Emmett, and Teller-plots (BET) was used to determine the specific surface area and pore size distribution of these matrices. It could be clearly shown, that variations in P/L ratio influenced both the porosity of cement and vancomycin release profiles. Antibiotic activity during release study was successfully measured using an agar diffusion assay. However, vancomycin-HCl encapsulation into PLGA polymer microspheres decreased porosity influence of cement on drug release while maintaining antibiotic activity of the embedded substance.

  10. Orbital floor reconstruction using calcium phosphate cement paste: an animal study.

    Science.gov (United States)

    Tañag, Marvin A; Yano, Kenji; Hosokawa, Ko

    2004-12-01

    Orbital floor defects were created in 10 New Zealand white rabbits and were reconstructed using an injectable calcium phosphate paste. These animals were euthanized at 2, 4, 8, and 12 months after implantation and were examined for biocompatibility and osteoconductivity. Grossly, implants were found to be adherent to the floor and covered with fibrous tissues. There was no sign of infection, extrusion, or migration of implant within the orbit and maxilla. The orbital floor was completely restored. Histological examination showed active new bone formation that encroached within the implant and gradually increased in density with time. Maxillary mucosa and glands were likewise reconstituted. Thin fibrovascular tissues were seen on top of and within the surface of the implant, and few to slight inflammatory cells were seen. Microradiography showed direct apposition between the new bone and the implant. These findings compare favorably with previously published reports on the biocompatibility and osteoconductivity of calcium phosphate cement. The authors believe that, together with ease of use and structural integrity, calcium phosphate paste can be useful in orbital floor reconstruction.

  11. Designing calcium phosphate-based bifunctional nanocapsules with bone-targeting properties

    Energy Technology Data Exchange (ETDEWEB)

    Khung, Yit-Lung; Bastari, Kelsen; Cho, Xing Ling; Yee, Wu Aik; Loo, Say Chye Joachim, E-mail: joachimloo@ntu.edu.sg [Nanyang Technological University, School of Materials Science and Engineering (Singapore)

    2012-06-15

    Using sodium dodecyl sulphate micelles as template, hollow-cored calcium phosphate nanocapsules were produced. The surfaces of the nanocapsule were subsequently silanised by a polyethylene glycol (PEG)-based silane with an N-hydroxysuccinimide ester end groups which permits for further attachment with bisphosphonates (BP). Characterisations of these nanocapsules were investigated using Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy, Fourier Transform Infra-Red Spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy and Dynamic Light Scattering. To further validate the bone-targeting potential, dentine discs were incubated with these functionalised nanocapsules. FESEM analysis showed that these surface-modified nanocapsules would bind strongly to dentine surfaces compared to non-functionalised nanocapsules. We envisage that respective components would give this construct a bifunctional attribute, whereby (1) the shell of the calcium phosphate nanocapsule would serve as biocompatible coating aiding in gradual osteoconduction, while (2) surface BP moieties, acting as targeting ligands, would provide the bone-targeting potential of these calcium phosphate nanocapsules.

  12. Calcium phosphate coating on magnesium alloy for modification of degradation behavior

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Magnesium alloy has similar mechanical properties with natural bone,but its high susceptibility to corrosion has limited its application in orthopedics.In this study,a calcium phosphate coating is formed on magnesium alloy (AZ31) to control its degradation rate and enhance its bioactivity and bone inductivity.Samples of AZ31 plate were placed in the supersaturated calcification solution prepared with Ca(NO3)2,NaH2PO4 and NaHCO3,then the calcium phosphate coating formed.Through adjusting the immersion time,the thickness of uniform coatings can be changed from 10 to 20 μm.The composition,phase structure and morphology of the coatings were investigated.Bonding strength of the coatings and substrate was 2-4 MPa in this study.The coatings significantly decrease degradation rate of the original Mg alloy,indicating that the Mg alloy with calcium phosphate coating is a promising degradable bone material.

  13. Development of a Calcium Phosphate Nanocomposite for Fast Fluorogenic Detection of Bacteria

    Directory of Open Access Journals (Sweden)

    Claudio R. Martínez

    2014-09-01

    Full Text Available Current procedures for the detection and identification of bacterial infections are laborious, time-consuming, and require a high workload and well-equipped laboratories. Therefore the work presented herein developed a simple, fast, and low cost method for bacterial detection based on hydroxyapatite nanoparticles with a nutritive mixture and the fluorogenic substrate. Calcium phosphate ceramic nanoparticles were characterized and integrated with a nutritive mixture for the early detection of bacteria by visual as well as fluorescence spectroscopy techniques. The composite was obtained by combining calcium phosphate nanoparticles (Ca:P ratio, 1.33:1 with a nutritive mixture of protein hydrolysates and carbon sources, which promote fast bacterial multiplication, and the fluorogenic substrate 4-methylumbellipheryl-β-d-glucuronide (MUG. The composite had an average particle size of 173.2 nm and did not show antibacterial activity against Gram-negative or Gram-positive bacteria. After an Escherichia coli suspension was in contact with the composite for 60–90 min, fluorescence detected under UV light or by fluorescence spectrophotometer indicated the presence of bacteria. Intense fluorescence was observed after incubation for a maximum of 90 min. Thus, this calcium phosphate nanocomposite system may be useful as a model for the development of other nanoparticle composites for detection of early bacterial adhesion.

  14. Cell response of calcium phosphate based ceramics, a bone substitute material

    Directory of Open Access Journals (Sweden)

    Juliana Marchi

    2013-01-01

    Full Text Available The aim of this study was to characterize calcium phosphate ceramics with different Ca/P ratios and evaluate cell response of these materials for use as a bone substitute. Bioceramics consisting of mixtures of hydroxyapatite (HAp and β-tricalcium phosphate (β-TCP powders in different proportions were pressed and sintered. The physical and chemical properties of these bioceramics were then characterized. Characterization of the biological properties of these materials was based on analysis of cell response using cultured fibroblasts. The number of cells attached to the samples was counted from SEM images of samples exposed to cell culture solution for different periods. These data were compared by analysis of variance (ANOVA complemented by the Tukey's test. The TCP sample had higher surface roughness and lower density. The adherence and growth of FMM1 cells on samples from all groups was studied. Even though the different calcium based ceramics exhibited properties which made them suitable as bone substitutes, those with higher levels of β-TCP revealed improved cell growth on their surfaces. These observations indicated two-phase calcium phosphate based materials with a β-TCP surface layer to be a promising bone substitute.

  15. 3D Printing of Composite Calcium Phosphate and Collagen Scaffolds for Bone Regeneration

    Science.gov (United States)

    Inzana, Jason A.; Olvera, Diana; Fuller, Seth M.; Kelly, James P.; Graeve, Olivia A.; Schwarz, Edward M.; Kates, Stephen L.; Awad, Hani A.

    2014-01-01

    Low temperature 3D printing of calcium phosphate scaffolds holds great promise for fabricating synthetic bone graft substitutes with enhanced performance over traditional techniques. Many design parameters, such as the binder solution properties, have yet to be optimized to ensure maximal biocompatibility and osteoconductivity with sufficient mechanical properties. This study tailored the phosphoric acid-based binder solution concentration to 8.75 wt% to maximize cytocompatibility and mechanical strength, with a supplementation of Tween 80 to improve printing. To further enhance the formulation, collagen was dissolved into the binder solution to fabricate collagen-calcium phosphate composites. Reducing the viscosity and surface tension through a physiologic heat treatment and Tween 80, respectively, enabled reliable thermal inkjet printing of the collagen solutions. Supplementing the binder solution with 1–2 wt% collagen significantly improved maximum flexural strength and cell viability. To assess the bone healing performance, we implanted 3D printed scaffolds into a critically sized murine femoral defect for 9 weeks. The implants were confirmed to be osteoconductive, with new bone growth incorporating the degrading scaffold materials. In conclusion, this study demonstrates optimization of material parameters for 3D printed calcium phosphate scaffolds and enhancement of material properties by volumetric collagen incorporation via inkjet printing. PMID:24529628

  16. Influence of polymeric additives on the cohesion and mechanical properties of calcium phosphate cements.

    Science.gov (United States)

    An, Jie; Wolke, Joop G C; Jansen, John A; Leeuwenburgh, Sander C G

    2016-03-01

    To expand the clinical applicability of calcium phosphate cements (CPCs) to load-bearing anatomical sites, the mechanical and setting properties of CPCs need to be improved. Specifically, organic additives need to be developed that can overcome the disintegration and brittleness of CPCs. Hence, we compared two conventional polymeric additives (i.e. carboxylmethylcellulose (CMC) and hyaluronan (HA)) with a novel organic additive that was designed to bind to calcium phosphate, i.e. hyaluronan-bisphosphonate (HABP). The unmodified cement used in this study consisted of a powder phase of α-tricalcium phosphate (α-TCP) and liquid phase of 4% NaH2PO4·2H2O, while the modified cements were fabricated by adding 0.75 or 1.5 wt% of the polymeric additive to the cement. The cohesion of α-TCP was improved considerably by the addition of CMC and HABP. None of the additives improved the compression and bending strength of the cements, but the addition of 0.75% HABP resulted into a significantly increased cement toughness as compared to the other experimental groups. The stimulatory effects of HABP on the cohesion and toughness of the cements is hypothesized to derive from the strong affinity between the polymer-grafted bisphosphonate ligands and the calcium ions in the cement matrix.

  17. Biomimetic synthesis of modified calcium phosphate fine powders and their in vitro studies

    Science.gov (United States)

    Gergulova, R.; Tepavitcharova, S.; Rabadjieva, D.; Sezanova, K.; Ilieva, R.; Alexandrova, R.; Andonova-Lilova, B.

    2013-12-01

    Biomimetic approach and subsequent high-temperature treatment were used to synthesize ion modified calcium phosphate fine powders. Thus, using Simulated Body Fluid (SBF) as an ion modifier, a bi-phase mixture of ion modified β-tricalcium phosphate and hydroxyapatite (β-TCP + HA) was prepared. The use of SBF electrolyte solution enriched with Mg2+ or Zn2+ yielded monophase β-tricalcium phosphate additionally modified with Mg2+ or Zn2+ (Mg-β-TCP or Zn-β-TCP). The in vitro behavior of the prepared powders on cell viability and proliferation of murine BALB/c 3T3 fibroblasts and of human Lep 3 cells was studied by MTT test assays and Mosmann method after 72 h incubation. The relative cell viability was calculated.

  18. Biomimetic synthesis of modified calcium phosphate fine powders and their in vitro studies

    Energy Technology Data Exchange (ETDEWEB)

    Gergulova, R., E-mail: rumigg@yahoo.com; Tepavitcharova, S., E-mail: rumigg@yahoo.com; Rabadjieva, D., E-mail: rumigg@yahoo.com; Sezanova, K., E-mail: rumigg@yahoo.com; Ilieva, R., E-mail: rumigg@yahoo.com [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., Bl. 11, 1113 Sofia (Bulgaria); Alexandrova, R.; Andonova-Lilova, B. [Institute of Experimental Morphology, Pathology and Anthropology with Museum, BAS, Acad. G. Bonchev Str., Bl. 25, Sofia (Bulgaria)

    2013-12-16

    Biomimetic approach and subsequent high-temperature treatment were used to synthesize ion modified calcium phosphate fine powders. Thus, using Simulated Body Fluid (SBF) as an ion modifier, a bi-phase mixture of ion modified β-tricalcium phosphate and hydroxyapatite (β-TCP + HA) was prepared. The use of SBF electrolyte solution enriched with Mg{sup 2+} or Zn{sup 2+} yielded monophase β-tricalcium phosphate additionally modified with Mg{sup 2+} or Zn{sup 2+} (Mg-β-TCP or Zn-β-TCP). The in vitro behavior of the prepared powders on cell viability and proliferation of murine BALB/c 3T3 fibroblasts and of human Lep 3 cells was studied by MTT test assays and Mosmann method after 72 h incubation. The relative cell viability was calculated.

  19. Effectiveness of nano-calcium phosphate paste on sensitivity during and after bleaching: a randomized clinical trial

    OpenAIRE

    LOGUERCIO, Alessandro Dourado; Lidia Yileng TAY; HERRERA,Daniel Rodrigo; Bauer,Jose; Reis, Alessandra

    2015-01-01

    The study aimed to evaluate the effectiveness of in-office bleaching and associated tooth sensitivity on application of nano-calcium phosphate paste as desensitizing agent. Bleaching was performed with 35% hydrogen peroxide gel in 40 patients who were randomly divided into placebo and nano-calcium phosphate paste groups. Bleaching efficacy (BE) was evaluated using a value-oriented Vita shade guide. Tooth sensitivity was recorded using a numeric rating scale (0–4) during bleaching and up...

  20. Elaboration de biocéramiques phosphocalciques Processing of calcium phosphate bioceramics

    Directory of Open Access Journals (Sweden)

    Champion Eric

    2013-11-01

    Full Text Available Les céramiques phosphocalciques (hydroxyapatite, phosphate tricalcique sont couramment utilisées comme implants synthétiques en substitution osseuse. Le développement de nouveaux implants céramiques aux performances accrues nécessite la maîtrise de nombreux paramètres chimiques et physiques intervenant dans leurs procédés d'élaboration : synthèse de poudres spécifiques, mise en forme d'architectures complexes contrôlées, frittage et fonctionnalisation. Cette contribution illustre à travers quelques exemples les travaux menés dans le domaine des procédés d'élaboration de ces biocéramiques phosphocalciques pour des applications en ingénierie des tissus osseux. Calcium phosphate ceramics (hydroxyapatite, tricalcium phosphate are commonly used as synthetic bone graft substitutes. The development of new ceramic implants with improved performances requires the mastering of many chemical and physical parameters involved in their processing: synthesis of specific powders, shaping of complex architectures, sintering and functionalization. This paper illustrates a few examples of the work in the field of processes of these calcium phosphate bioceramics for applications in bone tissue engineering.

  1. Brushite foams--the effect of Tween® 80 and Pluronic® F-127 on foam porosity and mechanical properties.

    Science.gov (United States)

    Unosson, Johanna; Montufar, Edgar B; Engqvist, Håkan; Ginebra, Maria-Pau; Persson, Cecilia

    2016-01-01

    Resorbable calcium phosphate based bone void fillers should work as temporary templates for new bone formation. The incorporation of macropores with sizes of 100 -300 µm has been shown to increase the resorption rate of the implant and speed up bone ingrowth. In this work, macroporous brushite cements were fabricated through foaming of the cement paste, using two different synthetic surfactants, Tween® 80 and Pluronic® F-127. The macropores formed in the Pluronic samples were both smaller and less homogeneously distributed compared with the pores formed in the Tween samples. The porosity and compressive strength (CS) were comparable to previously developed hydroxyapatite foams. The cement foam containing Tween, 0.5M citric acid in the liquid, 1 mass% of disodium dihydrogen pyrophosphate mixed in the powder and a liquid to powder ratio of 0.43 mL/g, showed the highest porosity values (76% total and 56% macroporosity), while the CS was >1 MPa, that is, the hardened cement could be handled without rupture of the foamed structure. The investigated brushite foams show potential for future clinical use, both as bone void fillers and as scaffolds for in vitro bone regeneration.

  2. The effect of some homopolymers on the crystallization of calcium phosphates

    Science.gov (United States)

    García-Ramos, J. V.; Carmona, P.

    1982-04-01

    Homopolymer additives (poly-L-glutamic acid, poly-L-aspartic acid and polyglycine) were examined for their effects on the crystallization of hydroxyapatite (HA) and brushite. An accelerating effect of poly-L-glutamic acid on the precipitation of HA and brushite was discovered, whereas polyacrylic acid accelerates preferentially the HA precipitation. This accelerating efficiency is shown to be correlated with structural factors. The crystal habit of HA is modified by adsorption of poly-L-aspartic acid, this habit becoming similar to that of HA crystals from renal stones.

  3. Identification of the hydrate gel phases present in phosphate-modified calcium aluminate binders

    Energy Technology Data Exchange (ETDEWEB)

    Chavda, Mehul A.; Bernal, Susan A. [Department of Materials Science and Engineering, The University of Sheffield, Sheffield S1 3JD (United Kingdom); Apperley, David C. [Solid-State NMR Group, Department of Chemistry, Durham University, Durham DH1 3LE (United Kingdom); Kinoshita, Hajime [Department of Materials Science and Engineering, The University of Sheffield, Sheffield S1 3JD (United Kingdom); Provis, John L., E-mail: j.provis@sheffield.ac.uk [Department of Materials Science and Engineering, The University of Sheffield, Sheffield S1 3JD (United Kingdom)

    2015-04-15

    The conversion of hexagonal calcium aluminate hydrates to cubic phases in hydrated calcium aluminate cements (CAC) can involve undesirable porosity changes and loss of strength. Modification of CAC by phosphate addition avoids conversion, by altering the nature of the reaction products, yielding a stable amorphous gel instead of the usual crystalline hydrate products. Here, details of the environments of aluminium and phosphorus in this gel were elucidated using solid-state NMR and complementary techniques. Aluminium is identified in both octahedral and tetrahedral coordination states, and phosphorus is present in hydrous environments with varying, but mostly low, degrees of crosslinking. A {sup 31}P/{sup 27}Al rotational echo adiabatic passage double resonance (REAPDOR) experiment showed the existence of aluminium–phosphorus interactions, confirming the formation of a hydrated calcium aluminophosphate gel as a key component of the binding phase. This resolves previous disagreements in the literature regarding the nature of the disordered products forming in this system.

  4. Enhanced biocorrosion resistance and biocompatibility of degradable Mg-Nd-Zn-Zr alloy by brushite coating.

    Science.gov (United States)

    Niu, Jialin; Yuan, Guangyin; Liao, Yi; Mao, Lin; Zhang, Jian; Wang, Yongping; Huang, Feng; Jiang, Yao; He, Yaohua; Ding, Wenjiang

    2013-12-01

    To further improve the corrosion resistance and biocompatibility of Mg-Nd-Zn-Zr alloy (JDBM), a biodegradable calcium phosphate coating (Ca-P coating) with high bonding strength was developed using a novel chemical deposition method. The main composition of the Ca-P coating was brushite (CaHPO4·2H2O). The bonding strength between the coating and the JDBM substrate was measured to be over 10 MPa, and the thickness of the coating layer was about 10-30 μm. The in vitro corrosion tests indicated that the Ca-P treatment improved the corrosion resistance of JDBM alloy in Hank's solution. Ca-P treatment significantly reduced the hemolysis rate of JDBM alloy from 48% to 0.68%, and induced no toxicity to MC3T3-E1 cells. The in vivo implantation experiment in New Zealand's rabbit tibia showed that the degradation rate was reduced obviously by the Ca-P treatment and less gas was produced from Ca-P treated JDBM bone plates and screws in early stage of the implantation, and at least 10weeks degradation time can be prolonged by the present coating techniques. Both Ca-P treated and untreated JDBM Mg alloy induced bone growth. The primary results indicate that the present Ca-P treatment is a promising technique for the degradable Mg-based biomaterials for orthopedic applications.

  5. The effect of Cu(II)-loaded brushite scaffolds on growth and activity of osteoblastic cells.

    Science.gov (United States)

    Ewald, Andrea; Käppel, Christine; Vorndran, Elke; Moseke, Claus; Gelinsky, Michael; Gbureck, Uwe

    2012-09-01

    Bone substitute materials such as calcium phosphate cements (CPC) are frequently used as growth factor carriers for the stimulation of osteoblast-formation around an implant. However, biological modification based on delicate protein factors like extracellular matrix proteins or growth factors is subject to a number of shortcomings like the need for storage below room temperature and cost of production. The aim of this study was to investigate ionic modification as an alternative bioinorganic route for implant modification. Although it is known that Cu(II) plays a role in angiogenesis and bone formation, not all involved processes are well understood yet. In this study the in vitro effect of Cu(II) on growth and activity of osteoblastic cells seeded on brushite (CaHPO(4) · 2 H(2) O) scaffolds as well as on glass discs was investigated. The results show that Cu(II) enhances cell activity and proliferation of osteoblastic cells on CPC and furthermore affects the expression of several bone specific proteins such as bone sialo protein or osteocalcin. Therefore, the modification of CPC with Cu(II) may offer a promising alternative to protein based modification to stimulate cellular activity for an improved bone healing.

  6. Changes in the drug release pattern of fresh and set simvastatin-loaded brushite cement.

    Science.gov (United States)

    Mestres, Gemma; Kugiejko, Karol; Pastorino, David; Unosson, Johanna; Öhman, Caroline; Karlsson Ott, Marjam; Ginebra, Maria-Pau; Persson, Cecilia

    2016-01-01

    Calcium phosphate cements are synthetic bone graft substitutes able to set at physiological conditions. They can be applied by minimally invasive surgery and can also be used as drug delivery systems. Consequently, the drug release pattern from the cement paste (fresh cement) is of high clinical interest. However, previous studies have commonly evaluated the drug release using pre-set cements only. Therefore, the aim of this work was to determine if the time elapsed from cement preparation until immersion in the solution (3 min for fresh cements, and 1h and 15 h for pre-set cements) had an influence on its physical properties, and correlating these to the drug release profile. Simvastatin was selected as a model drug, while brushite cement was used as drug carrier. This study quantified how the setting of a material reduces the accessibility of the release media to the material, thus preventing drug release. A shift in the drug release pattern was observed, from a burst-release for fresh cements to a sustained release for pre-set cements.

  7. Calcium phosphate flocs and the clarification of sugar cane juice from whole of crop harvesting.

    Science.gov (United States)

    Thai, Caroline C D; Moghaddam, Lalehvash; Doherty, William O S

    2015-02-11

    Sugar cane biomass is one of the most viable feedstocks for the production of renewable fuels and chemicals. Therefore, processing the whole of crop (WC) (i.e., stalk and trash, instead of stalk only) will increase the amount of available biomass for this purpose. However, effective clarification of juice expressed from WC for raw sugar manufacture is a major challenge because of the amounts and types of non-sucrose impurities (e.g., polysaccharides, inorganics, proteins, etc.) present. Calcium phosphate flocs are important during sugar cane juice clarification because they are responsible for the removal of impurities. Therefore, to gain a better understanding of the role of calcium phosphate flocs during the juice clarification process, the effects of impurities on the physicochemical properties of calcium phosphate flocs were examined using small-angle laser light scattering technique, attenuated total reflectance Fourier transformed infrared spectroscopy, and X-ray powder diffraction. Results on synthetic sugar juice solutions showed that the presence of SiO2 and Na(+) ions affected floc size and floc structure. Starch and phosphate ions did not affect the floc structure; however, the former reduced the floc size, whereas the latter increased the floc size. The study revealed that high levels of Na(+) ions would negatively affect the clarification process the most, as they would reduce the amount of suspended particles trapped by the flocs. A complementary study on prepared WC juice using cold and cold/intermediate liming techniques was conducted. The study demonstrated that, in comparison to the one-stage (i.e., conventional) clarification process, a two-stage clarification process using cold liming removed more polysaccharides (≤19%), proteins (≤82%), phosphorus (≤53%), and SiO2 (≤23%) in WC juice but increased Ca(2+) (≤136%) and sulfur (≤200%).

  8. Dissolution and storage stability of nanostructured calcium carbonates and phosphates for nutrition

    Science.gov (United States)

    Posavec, Lidija; Knijnenburg, Jesper T. N.; Hilty, Florentine M.; Krumeich, Frank; Pratsinis, Sotiris E.; Zimmermann, Michael B.

    2016-10-01

    Rapid calcium (Ca) dissolution from nanostructured Ca phosphate and carbonate (CaCO3) powders may allow them to be absorbed in much higher fraction in humans. Nanosized Ca phosphate and CaCO3 made by flame-assisted spray pyrolysis were characterized by nitrogen adsorption, X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscopy. As-prepared nanopowders contained both CaCO3 and CaO, but storing them under ambient conditions over 130 days resulted in a complete transformation into CaCO3, with an increase in both crystal and particle sizes. The small particle size could be stabilized against such aging by cation (Mg, Zn, Sr) and anion (P) doping, with P and Mg being most effective. Calcium phosphate nanopowders made at Ca:P ≤ 1.5 were XRD amorphous and contained γ-Ca2P2O7 with increasing hydroxyapatite content at higher Ca:P. Aging of powders with Ca:P = 1.0 and 1.5 for over 500 days gradually increased particle size (but less than for CaCO3) without a change in phase composition or crystallinity. In 0.01 M H3PO4 calcium phosphate nanopowders dissolved ≈4 times more Ca than micronsized compounds and about twice more Ca than CaCO3 nanopowders, confirming that nanosizing and/or amorphous structuring sharply increases Ca powder dissolution. Because higher Ca solubility in vitro generally leads to greater absorption in vivo, these novel FASP-made Ca nanostructured compounds may prove useful for nutrition applications, including supplementation and/or food fortification.

  9. The effects of calcium phosphate particles on the growth of osteoblasts.

    Science.gov (United States)

    Sun, J S; Tsuang, Y H; Liao, C J; Liu, H C; Hang, Y S; Lin, F H

    1997-12-01

    With advances in ceramics technology, calcium phosphate bioceramics have been applied as bone substitutes for several decades. The focus of this work is to elucidate the biocompatibility of the particulates of various calcium phosphate cytotoxicities. Four different kinds of calcium phosphate powders, including beta-tricalcium phosphate (beta-TCP), hydroxyapatite (HA), beta-dicalcium pyrophosphate (beta-DCP), and sintered beta-dicalcium pyrophosphate (SDCP), were tested by osteoblast cell culture. The results were analyzed by cell count, concentration of transforming growth factor-beta 1 (TGF-beta 1), alkaline phosphatase (ALP), and prostaglandin E2 (PGE2) in culture media. The changes were most significant when osteoblasts were cultured with beta-TCP and HA bioceramics. The changes in cell population of the beta-TCP and HA were quite low in the first 3 days, then increased gradually toward the seventh day. The changes in TGF-beta 1 concentration in culture medium inversely related to the changes in cell population. The ALP titer in the culture media of the beta-TCP and HA were quite high in the first 3 days, then decreased rapidly between the third and seventh days. The concentrations of PGE2 in the culture media tested were quite high on the first day, decreased rapidly to the third day, and then gradually until the seventh day. The changes in the beta-DCP and SDCP were quite similar to those of HA and beta-TCP but much less significant. We conclude that HA and beta-TCP have an inhibitory effect on the growth of osteoblasts. The inhibitins effects of the HA and beta-TCP powders on the osteoblast cell cultures possibly are mediated by the increased synthesis of PGE2.

  10. Glucose-6-phosphate reduces calcium accumulation in rat brain endoplasmic reticulum

    Directory of Open Access Journals (Sweden)

    Jeffrey Thomas Cole

    2012-04-01

    Full Text Available Brain cells expend large amounts of energy sequestering calcium (Ca2+, while loss of Ca2+ compartmentalization leads to cell damage or death. Upon cell entry, glucose is converted to glucose-6-phosphate (G6P, a parent substrate to several metabolic major pathways, including glycolysis. In several tissues, G6P alters the ability of the endoplasmic reticulum to sequester Ca2+. This led to the hypothesis that G6P regulates Ca2+ accumulation by acting as an endogenous ligand for sarco-endoplasmic reticulum calcium ATPase (SERCA. Whole brain ER microsomes were pooled from adult male Sprague-Dawley rats. Using radio-isotopic assays, 45Ca2+ accumulation was quantified following incubation with increasing amounts of G6P, in the presence or absence of thapsigargin, a potent SERCA inhibitor. To qualitatively assess SERCA activity, the simultaneous release of inorganic phosphate (Pi coupled with Ca2+ accumulation was quantified. Addition of G6P significantly and decreased Ca2+ accumulation in a dose-dependent fashion (1-10 mM. The reduction in Ca2+ accumulation was not significantly different that seen with addition of thapsigargin. Addition of glucose-1-phosphate or fructose-6-phosphate, or other glucose metabolic pathway intermediates, had no effect on Ca2+ accumulation. Further, the release of Pi was markedly decreased, indicating G6P-mediated SERCA inhibition as the responsible mechanism for reduced Ca2+ uptake. Simultaneous addition of thapsigargin and G6P did decrease inorganic phosphate in comparison to either treatment alone, which suggests that the two treatments have different mechanisms of action. Therefore, G6P may be a novel, endogenous regulator of SERCA activity. Additionally, pathological conditions observed during disease states that disrupt glucose homeostasis, may be attributable to Ca2+ dystasis caused by altered G6P regulation of SERCA activity

  11. Plasma Calcium, Inorganic Phosphate and Magnesium During Hypocalcaemia Induced by a Standardized EDTA Infusion in Cows

    Directory of Open Access Journals (Sweden)

    Enemark JMD

    2001-06-01

    Full Text Available The intravenous Na2EDTA infusion technique allows effective specific chelation of circulating Ca2+ leading to a progressive hypocalcaemia. Methods previously used were not described in detail and results obtained by monitoring total and free ionic calcium were not comparable due to differences in sampling and analysis. This paper describes a standardized EDTA infusion technique that allowed comparison of the response of calcium, phosphorus and magnesium between 2 groups of experimental cows. The concentration of the Na2EDTA solution was 0.134 mol/l and the flow rate was standardized at 1.2 ml/kg per hour. Involuntary recumbency occurred when ionised calcium dropped to 0.39 – 0.52 mmol/l due to chelation. An initial fast drop of ionized calcium was observed during the first 20 min of infusion followed by a fluctuation leading to a further drop until recumbency. Pre-infusion [Ca2+] between tests does not correlate with the amount of EDTA required to induce involuntary recumbence. Total calcium concentration measured by atomic absorption remained almost constant during the first 100 min of infusion but declined gradually when the infusion was prolonged. The concentration of inorganic phosphate declined gradually in a fluctuating manner until recumbency. Magnesium concentration remained constant during infusion. Such electrolyte responses during infusion were comparable to those in spontaneous milk fever. The standardized infusion technique might be useful in future experimental studies.

  12. The efficiency of child formula dentifrices containing different calcium and phosphate compounds on artificial enamel caries

    Science.gov (United States)

    Rirattanapong, Praphasri; Vongsavan, Kadkao; Saengsirinavin, Chavengkiat; Khumsub, Ploychompoo

    2016-01-01

    Objectives: Fluoride toothpaste has been extensively used to prevent dental caries. However, the risk of fluorosis is concerning, especially in young children. Calcium phosphate has been an effective remineralizing agent and is present in commercial dental products, with no risk of fluorosis to users. This in vitro study aimed to compare the effects of different calcium phosphate compounds and fluoride-containing dentifrices on artificial caries in primary teeth. Materials and Methods: Fifty sound primary incisors were coated with nail varnish, leaving two 1 mm2 windows on the labial surface before immersion in demineralizing solution for 96 hours to produce artificial enamel lesions. Subsequently, one window from each tooth was coated with nail varnish, and all 50 teeth were divided into five groups (n = 10); group A – deionized water; group B – casein phosphopeptide–amorphous calcium phosphate (CPP–ACP) paste (Tooth Mousse); group C – 500 ppm F (Colgate Spiderman®); group D – nonfluoridated toothpaste with triple calcium phosphate (Pureen®); and group E – tricalcium phosphate (TCP). Polarized light microscopy and Image-Pro® Plus software were used to evaluate lesions. Results: After a 7-day pH-cycle, mean lesion depths in groups A, B, C, D, and E had increased by 57.52 ± 10.66%, 33.28 ± 10.16%, 17.04 ± 4.76%, 32.51 ± 8.99%, and 21.76 ± 8.15%, respectively. All data were processed by the Statistical Package for the Social Sciences (version 16.0) software package. Comparison of percentage changes using one-way analysis of variance and Fisher's least squares difference tests at a 95% level of confidence demonstrated that group A was significantly different from the other groups (P < 0.001). Lesions in groups B and D had a significant lesion progression when compared with groups C and E. Conclusions: All toothpastes in this study had the potential to delay the demineralization progression of artificial enamel caries in primary teeth. The

  13. Synthesis and characterization of the aluminium phosphates modified with ammonium, calcium and molybdenum by hydrothermal method

    Directory of Open Access Journals (Sweden)

    Łuczka Kinga

    2016-06-01

    Full Text Available Synthesis and characterization of the aluminum phosphates modified with ammonium, calcium and molybdenum were conducted. The influence of process parameters (reactive pressure and molar ratios in the reaction mixture were studied. The contents of the individual components in the products were in the range of: 10.97–17.31 wt% Al, 2.65–13.32 wt% Ca, 0.70–3.11 wt% Mo, 4.36–8.38 wt% NH3, and 35.12–50.54 wt% P2O5. The materials obtained in the experiments were characterized by various physicochemical parameters. The absorption oil number was in the range from 67 to 89 of oil/100 g of product, the surface area was within the range of 4–76 m2/g, whereas the average particle size of products reached 282–370 nm. The Tafel tests revealed comparable anticorrosive properties of aluminum phosphates modified with ammonium, calcium, molybdenum in comparison with commercial phosphate.

  14. In Situ Laser Coating of Calcium Phosphate on TC4 Surface for Enhancing Bioactivity

    Institute of Scientific and Technical Information of China (English)

    DENG Chi; WANG Yong; ZHANG Ya-ping; GAO Jia-cheng

    2007-01-01

    Titanium alloy has been a successful implant material owing to its excellent ratio of strength to weight,toughness, and bio-inert oxide surface. Significant progress has been made in improving the bioactivity of titanium alloy by coating its oxide surface with calcium phosphates. In the present study, in situ coating was reported on Ti6Al4V(TC4) surface with calcium phosphate (Ca-P) bioceramics synthesized and synchronously cladded by laser beam. This coating was grown by first preplacing directly the raw powders, which contain 80% of CaHPO4 ·2H2O, 20% of CaCO3, and dram of rare earth (RE), on the TC4 surfaces, and then exposing the surfaces to the laser beam with a power density of 12. 73-15.27 MW · m-2 and a scanning velocity of 10. 5 m/s. The resultant coating was characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis and Different-thermal Scanning (TG-DSC), and Energy Dispersive X-ray Detection (EDX). The results show that these laser ceramics include hydroxyapatite (HA), tricalcium phosphate (TCP), Ca2P2O7, and other Ca-P phases, and the interface between the coating and the TC4 substrate has tighter fixation, in which the chemical bonding is approved. These laser hybrid coatings are useful in enhancing the bioactivity of titanium alloy surfaces.

  15. Influences of the steam sterilization on the properties of calcium phosphate porous bioceramics.

    Science.gov (United States)

    Li, Xiangfeng; Guo, Bo; Xiao, Yumei; Yuan, Tun; Fan, Yujiang; Zhang, Xingdong

    2016-01-01

    The influences of steam sterilization on the physicochemical properties of calcium phosphate (Ca-P) porous bioceramics, including β-tricalcium phosphate (β-TCP), biphasic calcium phosphate (BCP) and hydroxyapatite (HA) are investigated. After being steam sterilized in an autoclave (121 °C for 40 min), the porous bioceramics are dried and characterized. The steam sterilization has no obvious effects on the phase composition, thermal stability, pH value and dissolubility of β-TCP porous bioceramic, but changes its morphology and mechanical strength. Meanwhile, the steam sterilization leads to the significant changes of the morphology, phase composition, pH value and dissolubility of BCP porous bioceramic. The increase of dissolubility and mechanical strength, the decrease of pH value of the immersed solution and partial oriented growth of crystals are also observed in HA porous bioceramic after steam sterilization. These results indicate that the steam sterilization can result in different influences on the physicochemical properties of β-TCP, BCP and HA porous bioceramics, thus the application of the steam sterilization on the three kinds of Ca-P porous bioceramics should be considered carefully based on the above changed properties.

  16. Hemolysis effect and calcium-phosphate precipitation of heat-organic-film treated magnesium

    Institute of Scientific and Technical Information of China (English)

    GAO Jia-cheng; QIAO Li-ying; LI Long-chuan; WANG Yong

    2006-01-01

    A heat-organic-films process was employed to induce calcium-phosphate apatites formation on magnesium, consequently the corrosion resistance and hemolysis properties of magnesium were improved for biomedical applications. Firstly, magnesium samples were heat-treated at 773 K for 10 h; secondly, stearic acid films were coated on the surface of the heat-treated magnesium.Then the surface modified magnesium was soaked in simulated body fluid (SBF) to test its corrosion resistance. The results show that the heat treatment process allows magnesium to form a dense oxide layer with a thickness of around 20 μm, thereby the surface modified magnesium has higher corrosion resistance. After 24 h in SBF island apatite was deposited on magnesium. The unevenly precipitates were characterized by XRD and FTIR as the mixture of hydroxyapatite(HA) and octacalcium phosphate(OCP). The preliminary hemolysis experiment indicates that untreated magnesium has hemolytic effect (about 60%); whereas the heat-organic film treated samples has no hemolytic effect. The mechanism of fast nucleation and growth of calcium-phosphate apatites on surface modified magnesium in SBF was also discussed.

  17. Introduction of enzymatically degradable poly(trimethylene carbonate) microspheres into an injectable calcium phosphate cement.

    Science.gov (United States)

    Habraken, Wouter J E M; Zhang, Zheng; Wolke, Joop G C; Grijpma, Dirk W; Mikos, Antonios G; Feijen, Jan; Jansen, John A

    2008-06-01

    Poly(trimethylene carbonate) (PTMC) is an enzymatically degradable polyester with rubber-like properties. Introduction of this polymer into an injectable calcium phosphate bone cement can therefore be used to introduce macroporosity into the cement for tissue engineering purposes as well as to improve mechanical properties. Aim of this study was to investigate calcium phosphate cements with incorporated PTMC microspheres (PTMC CPCs) on their physical/mechanical properties and in vitro degradation characteristics. Therefore, composites were tested on setting time and mechanical strength as well as subjected to phosphate buffered saline (PBS) and enzyme containing medium. PTMC CPCs (12.5 and 25 wt%) with molecular weights of 52.7 kg mol(-1) and 176.2 kg mol(-1) were prepared, which showed initial setting times similar to that of original CPC. Though compression strength decreased upon incorporation of PTMC microspheres, elastic properties were improved as strain-at-yield increased with increasing content of microspheres. Sustained degradation of the microspheres inside PTMC CPC occurred when incubated in the enzymatic environment, but not in PBS, which resulted in an interconnected macroporosity for the 25 wt% composites.

  18. Composition of calcium phosphates precipitated from aqueous solutions at different pH values

    Energy Technology Data Exchange (ETDEWEB)

    Salahi, E.; Moztarzadeh, F. [Ceramics Div., Teheran (Iran). Materials and Energy Research Center

    2001-03-01

    During the preparation of calcium phosphate compounds by precipitation from aqueous solutions, several phases, namely dicalcium hydrogen phosphate (DCP, CaHPO{sub 4}), dicalcium hydrogen phosphate dihydrate DCPD, CaHPO{sub 4} (2 H{sub 2}O), hydrated calcium phosphate Ca{sub 3}(PO){sub 4} 2(H{sub 2}O) and hydroxyapatite (HAp, Ca10(PO{sub 4})6(OH){sub 2}), can be formed at different pH values. In the research work presented here, Ca(NO{sub 3})2(4H{sub 2}O) and (NH{sub 4})2HPO{sub 4} were used as starting materials The two solutions with an initial molar ratio of Ca/P=1,67 were mixed at 20 C at 0calcium phosphate are formed. A structural transition was observed at 8phosphate ({beta}-TCP,Ca{sub 3}(PO{sub 4}){sub 2}) developed. Between pH 8 and 9, this phase could be observed clearly. At pH 9..10, there is a transitional state, and at pH >10,5, the hydroxyapatite was developed completely. (orig.)

  19. Porous bioceramic bead prepared by calcium phosphate with sodium alginate gel and PE powder

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Y.C. [Department of Orthopaedic Surgery, Kaohsiung Medical University Hospital, Kaohsiung 807, Taiwan (China); Ho, M.L.; Wu, S.C. [Department of Physiology, Kaohsiung Medical University, 100, Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China); Hsieh, H.S. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100, Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China); Wang, C.K. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100, Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China)], E-mail: ckwang@kmu.edu.tw

    2008-08-01

    The porous calcium phosphate beads were made by an alginate-interacting Ca ions mechanism on addition of a pore-forming polyethylene (PE) powder at 1250 deg. C sintering. The nature of the powders and porous beads were analyzed through X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR) and heavy metal analysis by inductively coupled plasma-optical emission spectroscopy (ICP-OES). The porous beads size and the pore microstructure characteristics were determined using scanning electron microscopy (SEM). Beside, the porosity analysis was evaluated out using an Archimedes' principle and mercury porosimetry. Then, the sodium ampicillin was penetrated/adsorbed onto calcium-deficient hydroxyapatite porous beads, and was subsequently released in PBS. No matter whether the raw material was HAp, TCP or biphase, the Ca{sub 9}(HPO{sub 4})(PO{sub 4}){sub 5}OH phase (CDHA) was formed only after sintering. Porous beads of various calcium phosphates with different sizes (0.9-1.1 mm) and pore size groups (60-120 {mu}m and lower than 10 {mu}m) were appeared. The release kinetics of sodium ampicillin from these porous beads have indicated the possibility of using these materials as possible carriers for drug delivery.

  20. Single step preparation of nanosilver loaded calcium phosphate by low temperature co-conversion process.

    Science.gov (United States)

    Suwanprateeb, J; Thammarakcharoen, F; Wasoontararat, K; Chokevivat, W; Phanphiriya, P

    2012-09-01

    The preparation and characterization of nanosilver loaded calcium phosphate aiming to enhance the bactericidal performance by a single step co-conversion technique using low temperature ion exchange phosphorization in combination with Tollen's reaction were performed. Silver nitrate was used as a silver ion supply source (0.001-0.1 M) and glucose was employed as a reducing agent. After conversion, surface and shell zones of all samples comprised hydroxyapatite and metallic silver as the main phases regardless of silver nitrate concentration. However, hydroxyapatite, residual calcium sulfate and monetite were found in the core zone when using silver nitrate concentration lower than 0.1 M. The microstructure of all samples comprised the distribution of spherical-shaped silver nanoparticles within the cluster of calcium phosphate nanocrystals. Total silver content (range, 0.09-6.5 %) in the converted samples was found to linearly increase with increasing silver nitrate content. Flexural modulus and strength of converted samples generally decreased with increasing silver content. Effective antibacterial activity of two selected samples (0.001 and 0.005 M AgNO(3)) against two bacterial strains (Pseudomonas aeruginosa and Staphylococcus aureus) was observed. Cytotoxic potentials by MTT assay of both samples were observed at 24 and 48 h extraction respectively.

  1. Reactive calcium-phosphate-containing poly(ester-co-ether) methacrylate bone adhesives: chemical, mechanical and biological considerations.

    Science.gov (United States)

    Zhao, Xin; Olsen, Irwin; Li, Haoying; Gellynck, Kris; Buxton, Paul G; Knowles, Jonathan C; Salih, Vehid; Young, Anne M

    2010-03-01

    A poly(propylene glycol-co-lactide) dimethacrylate adhesive with monocalcium phosphate monohydrate (MCPM)/beta-tricalcium phosphate (beta-TCP) fillers in various levels has been investigated. Water sorption by the photo-polymerized materials catalyzed varying filler conversion to dicalcium phosphate (DCP). Polymer modulus was found to be enhanced upon raising total calcium phosphate content. With greater DCP levels, faster release of phosphate and calcium ions and improved buffering of polymer degradation products were observed. This could reduce the likelihood of pH-catalyzed bulk degradation and localized acid production and thereby may prevent adverse biological responses. Bone-like MG-63 cells were found to attach, spread and have normal morphology on both the polymer and composite surfaces. Moreover, composites implanted into chick embryo femurs became closely apposed to the host tissue and did not appear to induce adverse immunological reaction. The above results suggest that the new composite materials hold promise as clinical effective bone adhesives.

  2. The protective effect of supplemental calcium on colonic permeability depends on a calcium phosphate-induced increase in luminal buffering capacity.

    Science.gov (United States)

    Schepens, Marloes A A; ten Bruggencate, Sandra J M; Schonewille, Arjan J; Brummer, Robert-Jan M; van der Meer, Roelof; Bovee-Oudenhoven, Ingeborg M J

    2012-04-01

    An increased intestinal permeability is associated with several diseases. Previously, we have shown that dietary Ca decreases colonic permeability in rats. This might be explained by a calcium-phosphate-induced increase in luminal buffering capacity, which protects against an acidic pH due to microbial fermentation. Therefore, we investigated whether dietary phosphate is a co-player in the effect of Ca on permeability. Rats were fed a humanised low-Ca diet, or a similar diet supplemented with Ca and containing either high, medium or low phosphate concentrations. Chromium-EDTA was added as an inert dietary intestinal permeability marker. After dietary adaptation, short-chain fructo-oligosaccharides (scFOS) were added to all diets to stimulate fermentation, acidify the colonic contents and induce an increase in permeability. Dietary Ca prevented the scFOS-induced increase in intestinal permeability in rats fed medium- and high-phosphate diets but not in those fed the low-phosphate diet. This was associated with higher faecal water cytotoxicity and higher caecal lactate levels in the latter group. Moreover, food intake and body weight during scFOS supplementation were adversely affected by the low-phosphate diet. Importantly, luminal buffering capacity was higher in rats fed the medium- and high-phosphate diets compared with those fed the low-phosphate diet. The protective effect of dietary Ca on intestinal permeability is impaired if dietary phosphate is low. This is associated with a calcium phosphate-induced increase in luminal buffering capacity. Dragging phosphate into the colon and thereby increasing the colonic phosphate concentration is at least part of the mechanism behind the protective effect of Ca on intestinal permeability.

  3. Proliferation and differentiation of osteoblast-like MC3T3-E1 cells on biomimetically and electrolytically deposited calcium phosphate coatings

    NARCIS (Netherlands)

    Wang, Jiawei; Boer, de Jan; Groot, de Klaas

    2008-01-01

    Biomimetic and electrolytic deposition are versatile methods to prepare calcium phosphate coatings. In this article, we compared the effects of biomimetically deposited octacalcium phosphate and carbonate apatite coatings as well as electrolytically deposited carbonate apatite coating on the prolife

  4. Continuous cellularization of calcium phosphate hybrid scaffolds induced by plasma polymer activation.

    Science.gov (United States)

    Bergemann, Claudia; Cornelsen, Matthias; Quade, Antje; Laube, Thorsten; Schnabelrauch, Matthias; Rebl, Henrike; Weißmann, Volker; Seitz, Hermann; Nebe, Barbara

    2016-02-01

    The generation of hybrid materials based on β-tricalcium phosphate (TCP) and various biodegradable polymers like poly(l-lactide-co-d,l-lactide) (PLA) represents a common approach to overcoming the disadvantages of pure TCP devices. These disadvantages lie in TCP's mechanical properties, such as brittleness. The positive characteristic of PLA - improvement of compressive strength of calcium phosphate scaffolds - is diametrically opposed to its cell attractiveness. Therefore, the objective of this work was to optimize osteoblast migration and cellularization inside a three-dimensionally (3D) printed, PLA polymer stabilized TCP hybrid scaffold by a plasma polymer process depositing amino groups via allylamine. MG-63 osteoblastic cells inside the 10mm hybrid scaffold were dynamically cultivated for 14days in a 3D model system integrated in a perfusion reactor. The whole TCP/PLA hybrid scaffold was continuously colonized due to plasma polymerized allylamine activation inducing the migration potential of osteoblasts.

  5. In situ synthesis of calcium phosphate-polycaprolactone nanocomposites with high ceramic volume fractions.

    Science.gov (United States)

    Makarov, C; Gotman, I; Jiang, X; Fuchs, S; Kirkpatrick, C J; Gutmanas, E Y

    2010-06-01

    Biodegradable calcium phosphate-PCL nanocomposite powders with unusually high ceramic volume fractions (80-95%) and uniform PCL distribution were synthesized by a non-aqueous chemical reaction in the presence of the dissolved polymer. No visible polymer separation occurred during processing. Depending on the reagents combination, either dicalcium phosphate (DCP) or Ca-deficient HA (CDHA) was obtained. CDHA-PCL composite powders were high pressure consolidated at room temperature yielding dense materials with high compressive strengths. Such densification route provides the possibility of incorporating drug and proteins without damaging their biological activity. The CDHA-PCL composites were tested in osteoblastic and endothelial cell line cultures and were found to support the attachment and proliferation of both cell types.

  6. Ultrastructural Analysis on the Osteogenesis and Transformation of Calcium Phosphate Ceramics in Vivo

    Institute of Scientific and Technical Information of China (English)

    Honglian DAI; Shipu LI; Yuhua YAN; Xianying CAO; Xuehui LU; Yang LENG

    2004-01-01

    To study the osteogenesis and transformation process of calcium phosphate bioceramic in vivo, biodegradable porous β-tricalcium phosphate ceramics (β-TCP, φ5×8 mm) were implanted in the tibia of rabbits. β-TCP ceramics with surrounding bone tissue were retrieved and observed by SEM, TEM and EPMA every month after implantation.The results showed that osteogenesis was active and β-TCP ceramics bonded to bones directly. The new bones were forming and maturing as materials were continuously degrading, and materials were finally replaced by new bone. Parts of the materials were degraded, absorbed and recrystallized, while the rest were dispersed to the spongy bone and the Haversian lamella in an irregular arrangement, becoming incorporated into bone formation directly by remodeling the structure. Some β-TCP crystals cleaved along its (001) rhombohedral plane and formed lath-like crystals in vivo.

  7. Preparation of Laminin-apatite-polymer Composites Using Metastable Calcium Phosphate Solutions

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    A synthetic polymer with a laminin-apatite composite layer on its surface would be useful as a percutaneous device. The preparation of such a composite was attempted in the present study using poly ( ethylene terephthalate ) (PET) and polyethylene ( PE ) as the synthetic polymer. PET and PE plates and those pretreated with an oxygen plasma were alternately dipped in calcium and phosphate ion solutions, and then immersed in a metastable ealcium phosphate solution supplemented with laminin ( LCP solution ). The PET and PE plates pretreated with an oxygen plasma formed a uniform and continuous layer of a laminin- apatite composite on their surfaces. In contrast, the PET and PE plates that had not been pretreated with an oxygen plasma did not form a continuous layer of a laminin-apatite composite on their surfaces. The hydrophilic functional groups on the PET and PE surfaces introduced by the plasma treatment were responsible for the successful laminin-apatite composite coating.

  8. Injectable Hydrogel Composite Based Gelatin-PEG and Biphasic Calcium Phosphate Nanoparticles for Bone Regeneration

    Science.gov (United States)

    Van, Thuy Duong; Tran, Ngoc Quyen; Nguyen, Dai Hai; Nguyen, Cuu Khoa; Tran, Dai Lam; Nguyen, Phuong Thi

    2016-05-01

    Gelatin hydrogels have recently attracted much attention for tissue regeneration because of their biocompatibility. In this study, we introduce poly-ethylene glycol (PEG)—grafted gelatin containing tyramine moieties which have been utilized for in situ enzyme-mediated hydrogel preparation. The hydrogel can be used to load nanoparticles of biphasic calcium phosphate, a mixture of hydroxyapatite and β-tricalcium phosphate, and forming injectable bio-composites. Proton nuclear magnetic resonance (1H NMR) spectra indicated that tyramine-functionalized polyethylene glycol-nitrophenyl carbonate ester was conjugated to the gelatin. The hydrogel composite was rapidly formed in situ (within a few seconds) in the presence of horseradish peroxidase and hydrogen peroxide. In vitro experiments with bio-mineralization on the hydrogel composite surfaces was well-observed after 2 weeks soaking in simulated body fluid solution. The obtained results indicated that the hydrogel composite could be a potential injectable material for bone regeneration.

  9. Calcium phosphate/microgel composites for 3D powderbed printing of ceramic materials.

    Science.gov (United States)

    Birkholz, Mandy-Nicole; Agrawal, Garima; Bergmann, Christian; Schröder, Ricarda; Lechner, Sebastian J; Pich, Andrij; Fischer, Horst

    2016-06-01

    Composites of microgels and calcium phosphates are promising as drug delivery systems and basic components for bone substitute implants. In this study, we synthesized novel composite materials consisting of pure β-tricalcium phosphate and stimuli-responsive poly(N-vinylcaprolactam-co-acetoacetoxyethyl methacrylate-co-vinylimidazole) microgels. The chemical composition, thermal properties and morphology for obtained composites were extensively characterized by Fourier transform infrared, X-ray photoelectron spectroscopy, IGAsorp moisture sorption analyzer, thermogravimetric analysis, granulometric analysis, ESEM, energy dispersive X-ray spectroscopy and TEM. Mechanical properties of the composites were evaluated by ball-on-three-balls test to determine the biaxial strength. Furthermore, initial 3D powderbed-based printing tests were conducted with spray-dried composites and diluted 2-propanol as a binder to evaluate a new binding concept for β-tricalcium phosphate-based granulates. The printed ceramic bodies were characterized before and after a sintering step by ESEM. The hypothesis that the microgels act as polymer adhesive agents by efficient chemical interactions with the β-tricalcium phosphate particles was confirmed. The obtained composites can be used for the development of new scaffolds.

  10. The Properties of Sintered Calcium Phosphate with [Ca]/[P] = 1.50

    Directory of Open Access Journals (Sweden)

    Moo-Chin Wang

    2012-10-01

    Full Text Available In order to obtain the properties of the sintered as-dried calcium phosphate with [Ca]/[P] = 1.50, the characteristics of sintered pellets have been investigated using X-ray diffraction (XRD, inductively coupled plasma-mass spectrometry (ICP-MS, Fourier-transform infrared (FT-IR spectra, Vickers hardness indentation and scanning electron microscopy (SEM. When the pellet samples were sintered between 700 °C and 1200 °C for 4 h, the hydroxyapatite (Ca10(PO46(OH2, HA still maintained the major phase, accompanied with the rhenanite (NaCaPO4 as the secondary phase and β-tricalcium phosphate (β-Ca3(PO42, β-TCP as the minor phases. In addition, the HA partially transformed to α-tricalcium phosphate (α-Ca3(PO42, α-TCP and tetracalcium phosphate (Ca4(PO42O, TTCP, when the pellet samples were sintered at 1300 °C and 1400 °C, respectively, for 4 h. The maximum density and Vickers Hardness (HV of sintered pellet samples were 2.85 g/cm3 (90.18% theoretical density (T.D. and 407, which appeared at 1200 °C and 900 °C, respectively.

  11. Polymeric-Calcium Phosphate Cement Composites-Material Properties: In Vitro and In Vivo Investigations

    Science.gov (United States)

    Khashaba, Rania M.; Moussa, Mervet M.; Mettenburg, Donald J.; Rueggeberg, Frederick A.; Chutkan, Norman B.; Borke, James L.

    2010-01-01

    New polymeric calcium phosphate cement composites (CPCs) were developed. Cement powder consisting of 60 wt% tetracalcium phosphate, 30 wt% dicalcium phosphate dihydrate, and 10 wt% tricalcium phosphate was combined with either 35% w/w poly methyl vinyl ether maleic acid or polyacrylic acid to obtain CPC-1 and CPC-2. The setting time and compressive and diametral tensile strength of the CPCs were evaluated and compared with that of a commercial hydroxyapatite cement. In vitro cytotoxicity and in vivo biocompatibility of the two CPCs and hydroxyapatite cement were assessed. The setting time of the cements was 5–15 min. CPC-1 and CPC-2 showed significantly higher compressive and diametral strength values compared to hydroxyapatite cement. CPC-1 and CPC-2 were equivalent to Teflon controls after 1 week. CPC-1, CPC-2, and hydroxyapatite cement elicited a moderate to intense inflammatory reaction at 7 days which decreased over time. CPC-1 and CPC-2 show promise for orthopedic applications. PMID:20811498

  12. Polymeric-Calcium Phosphate Cement Composites-Material Properties: In Vitro and In Vivo Investigations

    Directory of Open Access Journals (Sweden)

    Rania M. Khashaba

    2010-01-01

    Full Text Available New polymeric calcium phosphate cement composites (CPCs were developed. Cement powder consisting of 60 wt% tetracalcium phosphate, 30 wt% dicalcium phosphate dihydrate, and 10 wt% tricalcium phosphate was combined with either 35% w/w poly methyl vinyl ether maleic acid or polyacrylic acid to obtain CPC-1 and CPC-2. The setting time and compressive and diametral tensile strength of the CPCs were evaluated and compared with that of a commercial hydroxyapatite cement. In vitro cytotoxicity and in vivo biocompatibility of the two CPCs and hydroxyapatite cement were assessed. The setting time of the cements was 5–15 min. CPC-1 and CPC-2 showed significantly higher compressive and diametral strength values compared to hydroxyapatite cement. CPC-1 and CPC-2 were equivalent to Teflon controls after 1 week. CPC-1, CPC-2, and hydroxyapatite cement elicited a moderate to intense inflammatory reaction at 7 days which decreased over time. CPC-1 and CPC-2 show promise for orthopedic applications.

  13. Synthesis and characterization of Ag-containing calcium phosphates with various Ca/P ratios

    Energy Technology Data Exchange (ETDEWEB)

    Gokcekaya, Ozkan, E-mail: gokcekaya@dc.tohoku.ac.jp [Department of Materials Processing, Tohoku University, 6-6-02 Aza Aoba, Aramaki, Aoba-ku, Sendai, Miyagi 980-8579 (Japan); Ueda, Kyosuke; Narushima, Takayuki [Department of Materials Processing, Tohoku University, 6-6-02 Aza Aoba, Aramaki, Aoba-ku, Sendai, Miyagi 980-8579 (Japan); Ergun, Celaletdin [Faculty of Mechanical Engineering, Istanbul Technical University, 65 Inonu Street, Gumussuyu, Istanbul 34437 (Turkey)

    2015-08-01

    Ag-containing calcium phosphate (CaP) powders were synthesized by a precipitation method using aqueous solutions of calcium nitrate, silver nitrate, and ammonium phosphate. The powders were sintered at temperatures ranging from 1173 to 1473 K. The charged atomic ratios of (Ca + Ag)/P and Ag/(Ca + Ag) in solution were varied from 1.33 to 1.67 and from 0 to 0.30, respectively. The Ag content in the as-precipitated CaP powders increased with the charged Ag/(Ca + Ag) atomic ratio in solution and was lower than the charged Ag/(Ca + Ag) value. The as-precipitated CaP powders consisted of hydroxyapatite (HA) as the main phase. Ag nanoparticles were observed on the as-precipitated HA particles under all conditions of Ag addition. After the sintering, HA, β-TCP (tricalcium phosphate), α-TCP, and β-CPP (calcium pyrophosphate) were mainly detected as CaPs on the basis of the Ca/P atomic ratio of the as-precipitated powders. The addition of Ag stabilized the β-TCP phase, and the distribution of Ag in β-TCP was homogeneous. A metallic Ag phase coexisted with HA. The solubility of Ag in HA was estimated to be 0.0019–0.0061 (Ag/(Ca + Ag)) atomic ratio, which was lower than that in β-TCP (higher than 0.0536) and higher than that of β-CPP (below the detection limit of analyses). - Highlights: • The HA powders with Ag nanoparticles were synthesized by a precipitation method. • Metallic Ag particles were detected with the HA phase after sintering. • The distribution of Ag in β-TCP was homogeneous after sintering. • The addition of Ag stabilized the β-ΤCP phase. • β-TCP exhibited higher solubility of Ag than HA and β-CPP.

  14. Direct 3D powder printing of biphasic calcium phosphate scaffolds for substitution of complex bone defects.

    Science.gov (United States)

    Castilho, Miguel; Moseke, Claus; Ewald, Andrea; Gbureck, Uwe; Groll, Jürgen; Pires, Inês; Teßmar, Jörg; Vorndran, Elke

    2014-03-01

    The 3D printing technique based on cement powders is an excellent method for the fabrication of individual and complex bone substitutes even in the case of large defects. The outstanding bone remodeling capacity of biphasic calcium phosphates (BCPs) containing hydroxyapatite (HA) as well as tricalcium phosphate (TCP) in varying ratios makes the adaption of powder systems resulting in BCP materials to this fabrication technique a desirable aim. This study presents the synthesis and characterization of a novel powder system for the 3D printing process, intended for the production of complexly shaped BCP scaffolds by a hydraulic setting reaction of calcium carbonate and TCP with phosphoric acid. The HA/TCP ratio in the specimens could be tailored by the calcium/phosphate ratio of the starting powder. The scaffolds could be fabricated with a dimensional accuracy of >96.5% and a minimal macro pore size of 300 µm. Independent of the phase composition the printed specimens showed a microporosity of approximately 68%, while the compressive strength strongly depended on the chemical composition and increased with rising TCP content in the scaffolds to a maximum of 1.81 MPa. Post-treatment of the scaffolds with a polylactic-co-glycolic acid-solution enhanced the mechanical properties by a factor of 8. In vitro studies showed that all BCP scaffolds were cytocompatible and enhanced the cell viability as well as the cell proliferation, as compared with pure TCP. Cell proliferation is even better on BCP when compared to HA and cell viability is in a similar range on these materials.

  15. Synthesis of calcium phosphates and porous hydroxyapatite beads prepared by emulsion method

    Energy Technology Data Exchange (ETDEWEB)

    Chen, B.-H. [Faculty of Biotechnology, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Chen, K.-I [Department of Electronics Engineering and Computer Science, Tung-Fang Institute of Technology, 100 Dungfang Road, Hunei, Kaohsiung, Taiwan (China); Ho, M.-L. [Department of Physiology, Kaohsiung Medical University, Kaohsiung 807, Taiwan (China); Chen, H.-N. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Chen, W.-C. [Faculty of Dentistry, Kaohsiung Medical University, Kaohsiung 807, Taiwan (China); Wang, C.-K. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China)], E-mail: ckwang@kmu.edu.tw

    2009-01-15

    Raw calcium phosphates were synthesized via a chemical reaction between 0.5 M orthophosphoric acid and 0.5 M calcium hydroxide. Hydroxyapatite (HAp), {beta}-tricalcium phosphate ({beta}-TCP) or biphase calcium phosphate (BCP) comprising HAp and {beta}-TCP were obtained by changing pH value, Ca/P ratio, and the addition of glycerol. The as-synthesized and heat-treated powders were analyzed by X-ray diffraction (XRD) and Fourier transformation infrared spectrometry (FTIR). Thermal stability of the pure apatite phase was obtained to be 1300 deg. C, while synthesis was done at the pH value of 10.0 with a Ca/P ratio of 2.0 and a temperature of 37 deg. C. Besides, the {beta}-TCP phase (with higher purity) was achieved at 800 deg. C, whose synthesis was done at pH 6.4 with a Ca/P ratio of 1.5 and a temperature of 37 deg. C. Therefore, the biphase bioceramics comprising of HAp and {beta}-TCP could be obtained, since it was manipulated suitably. The HAp raw material was subjected to a simple emulsion method for the preparation of porous beads. They should have the advantage of exhibiting higher adsorptive ability and osteoconductivity in comparison with the sintered dense apatite. Additionally, the porous beads of apatite were demonstrated to be non-toxic to cells, and should be suitable for the use as a scaffold of cultured bone and bone graft material, as well as for drug delivery systems.

  16. Biomimetic Precipitation of Uniaxially Grown Calcium Phosphate Crystals from Full-Length Human Amelogenin Sols

    Institute of Scientific and Technical Information of China (English)

    Vuk Uskokovié; Wu Li; Stefan Habelitz

    2011-01-01

    Human dental enamel forms over a period of 2 - 4 years by substituting the enamel matrix, a protein gel mostly composed of a single protein, amelogenin with fibrous apatite nanocrystals. Self-assembly of a dense amelogenin matrix is presumed to direct the growth of apatite fibers and their organization into bundles that eventually comprise the mature enamel, the hardest tissue in the mammalian body. This work aims to establish the physicochemical and biochemical conditions for the synthesis of fibrous apatite crystals under the control of a recombinant full-length human amelogenin matrix in combination with a programmable titration system. The growth of apatite substrates was initiated from supersaturated calcium phosphate solutions in the presence of dispersed amelogenin assemblies. It was shown earlier and confirmed in this study that binding of amelogenin onto apatite surfaces presents the first step that leads to substrate-specific crystal growth. In this work, we report enhanced nucleation and growth under conditions at which amelogenin and apatite carry opposite charges and adsorption of the protein onto the apatite seeds is even more favored. Experiments at pH below the isoelectric point of amelogenin showed increased protein binding to apatite and at low Ca/P molar ratios resulted in a change in crystal morphology from plate-like to fibrous and rod-shaped. Concentrations of calcium and phosphate ions in the supernatant did not show drastic decreases throughout the titration period, indicating controlled precipitation from the protein suspension metastable with respect to calcium phosphate. It is argued that ameloblasts in the developing enamel may vary the density of the protein matrix at the nano scale by varying local pH, and thus control the interaction between the mineral and protein phases. The biomimetic experimental setting applied in this study has thus proven as convenient for gaining insight into the fundamental nature of the process of

  17. Determinants of Brushite Stone Formation: A Case-Control Study

    OpenAIRE

    2013-01-01

    PURPOSE: The occurrence of brushite stones has increased during recent years. However, the pathogenic factors driving the development of brushite stones remain unclear. METHODS: Twenty-eight brushite stone formers and 28 age-, sex- and BMI-matched healthy individuals were enrolled in this case-control study. Anthropometric, clinical, 24 h urinary parameters and dietary intake from 7-day weighed food records were assessed. RESULTS: Pure brushite stones were present in 46% of patients, while ca...

  18. Effect of polydopamine on the biomimetic mineralization of mussel-inspired calcium phosphate cement in vitro

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Zongguang [Key Lab of Advanced Technologies of Materials, Ministry of Education, School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China); Qu, Shuxin, E-mail: qushuxin@swjtu.edu.cn [Key Lab of Advanced Technologies of Materials, Ministry of Education, School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China); Zheng, Xiaotong; Xiong, Xiong [Key Lab of Advanced Technologies of Materials, Ministry of Education, School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China); Fu, Rong; Tang, Kuangyun; Zhong, Zhendong [Department of Plastic Surgery, Academy of Medical Sciences and Sichuan Provincial People' s Hospital, Chengdu 610041 (China); Weng, Jie [Key Lab of Advanced Technologies of Materials, Ministry of Education, School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China)

    2014-11-01

    Inspired by the excellent adhesive property of mussel adhesive protein, we added polydopamine (PDA) to calcium phosphate cement (PDA–CPC) to enhance its compressive strength previously. The mineralization and mechanism on PDA–CPC were investigated by soaking it in simulated body fluid in this study. The results indicated that PDA promoted the conversion of dicalcium phosphate dihydrate and α-tricalcium phosphate to hydroxyapatite (HA) in the early stage but inhibited this conversion subsequently. PDA promoted the rapid mineralization on PDA–CPC to form a layer of nanoscale calcium phosphate (CaP) whereas there was no CaP formation on the control-CPC after 1 d of soaking. This layer of nanoscale CaP was similar to that of natural bone, which was always observed during soaking. X-ray photoelectron spectroscopy showed that the peak of C=O of PDA existed in the newly formed CaP on PDA–CPC, indicating the co-precipitation of CaP with PDA. Furthermore, the newly formed CaP on PDA–CPC was HA confirmed by transmission electron microscopy, which the newly formed HA was in association with PDA. Therefore, PDA increased the capacity of mineralization of CPC and induced the formation of nanoscale bone-like apatite on PDA–CPC. Thus, this provides the feasible route for surface modification on CPC. - Highlights: • Effect of polydopamine (PDA) on the in vitro mineralization of PDA-CPC was studied. • PDA promoted the rapid mineralization on PDA-CPC to form a nanoscale HA layer. • The precipitation of the nanoscale HA layer on PDA-CPC accompanied with PDA. • Polydopamine induced mineralization is feasible for surface modification of CaP.

  19. Alendronate-Eluting Biphasic Calcium Phosphate (BCP Scaffolds Stimulate Osteogenic Differentiation

    Directory of Open Access Journals (Sweden)

    Sung Eun Kim

    2015-01-01

    Full Text Available Biphasic calcium phosphate (BCP scaffolds have been widely used in orthopedic and dental fields as osteoconductive bone substitutes. However, BCP scaffolds are not satisfactory for the stimulation of osteogenic differentiation and maturation. To enhance osteogenic differentiation, we prepared alendronate- (ALN- eluting BCP scaffolds. The coating of ALN on BCP scaffolds was confirmed by scanning electron microscopy (FE-SEM, energy-dispersive X-ray spectroscopy (EDS, and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR. An in vitro release study showed that release of ALN from ALN-eluting BCP scaffolds was sustained for up to 28 days. In vitro results revealed that MG-63 cells grown on ALN-eluting BCP scaffolds exhibited increased ALP activity and calcium deposition and upregulated gene expression of Runx2, ALP, OCN, and OPN compared with the BCP scaffold alone. Therefore, this study suggests that ALN-eluting BCP scaffolds have the potential to effectively stimulate osteogenic differentiation.

  20. Postextraction socket grafting using calcium phosphate cement and platelet rich fibrin

    Directory of Open Access Journals (Sweden)

    Nihal Devkar

    2014-01-01

    Full Text Available This clinical case report describes and demonstrates the successful use of calcium phosphate cement (CPC in conjunction with platelet-rich fibrin (PRF for postextraction socket grafting in maxillary right first premolar area. CPC can be molded to form a scaffold. It has been used previously for regeneration in intrabony defects, but very few clinical studies in humans have reported its use for socket grafting. In this report, we have presented a novel use of CPC in conjunction with PRF for ridge preservation after tooth extraction.

  1. Ionic liquid-assisted formation of cellulose/calcium phosphate hybrid materials

    Science.gov (United States)

    Salama, Ahmed; Neumann, Mike; Günter, Christina

    2014-01-01

    Summary Cellulose/calcium phosphate hybrid materials were synthesized via an ionic liquid-assisted route. Scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, infrared spectroscopy, and thermogravimetric analysis/differential thermal analysis show that, depending on the reaction conditions, cellulose/hydroxyapatite, cellulose/chlorapatite, or cellulose/monetite composites form. Preliminary studies with MC3T3-E1 pre-osteoblasts show that the cells proliferate on the hybrid materials suggesting that the ionic liquid-based process yields materials that are potentially useful as scaffolds for regenerative therapies. PMID:25247137

  2. Ionic liquid-assisted formation of cellulose/calcium phosphate hybrid materials

    Directory of Open Access Journals (Sweden)

    Ahmed Salama

    2014-09-01

    Full Text Available Cellulose/calcium phosphate hybrid materials were synthesized via an ionic liquid-assisted route. Scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, infrared spectroscopy, and thermogravimetric analysis/differential thermal analysis show that, depending on the reaction conditions, cellulose/hydroxyapatite, cellulose/chlorapatite, or cellulose/monetite composites form. Preliminary studies with MC3T3-E1 pre-osteoblasts show that the cells proliferate on the hybrid materials suggesting that the ionic liquid-based process yields materials that are potentially useful as scaffolds for regenerative therapies.

  3. Si-TCP Synthesized from "Mg-free" Reagents Employed as Calcium Phosphate Cement

    OpenAIRE

    Mariana Motisuke; Raul García Carrodeguas; Cecília Amélia Carvalho Zavaglia

    2012-01-01

    The influence of silicon doping on calcium phosphate cement were explored in this work. α-TCP and Si-α-TCP were prepared by solid state reaction employing "Mg-free" CaHPO4, CaCO3 and CaSiO3 as precursors. It was possible to obtain TCP powders with low contents of β phase as contaminant. Cement liquid phase was an aqueous solution containing 2.5 wt. (%) of Na2HPO4 and 1.5 wt. (%) of citric acid. The liquid-to-powder ratio was 0.6 mL.g-1. Chemical, physical and mechanical propert...

  4. Effect of biomolecules from human renal matrix of calcium oxalate monohydrate (CaOx stones on in vitro calcium phosphate crystallization

    Directory of Open Access Journals (Sweden)

    Priyadarshini Pathak

    2010-10-01

    Full Text Available PURPOSE: Investigate the activity of high and low molecular weight biomolecules present in the matrix of human calcium oxalate (CaOx stones not only on the initial mineral phase formation of calcium and phosphate (CaP but also on its growth and demineralization of the preformed mineral phase. MATERIALS AND METHODS: Surgically removed renal stones were analyzed by Fourier Transform Infra Red (FTIR spectroscopy and only CaOx stones were extracted with 0.05M EGTA, 1 mM PMSF and 1% ß-mercaptoethanol. Renal CaOx stone extract was separated into > 10 kDa and 10 kDa and 10 kDa fraction lane. CONCLUSION: Both high and low molecular weight biomolecules extracted from human renal matrix of calcium oxalate (CaOx stones have a significant influence on calcium and phosphate (CaP crystallization.

  5. Effects of phosphates on microstructure and bioactivity of micro-arc oxidized calcium phosphate coatings on Mg-Zn-Zr magnesium alloy.

    Science.gov (United States)

    Pan, Y K; Chen, C Z; Wang, D G; Zhao, T G

    2013-09-01

    Calcium phosphate (CaP) coatings were prepared on Mg-Zn-Zr magnesium alloy by micro-arc oxidation (MAO) in electrolyte containing calcium acetate monohydrate (CH3COO)2Ca·H2O) and different phosphates (i.e. disodium hydrogen phosphate dodecahydrate (Na2HPO4·12H2O), sodium phosphate (Na3PO4·H2O) and sodium hexametaphosphate((NaPO3)6)). Scanning electron microscope (SEM), energy-dispersive X-ray spectrometry (EDS) and X-ray diffractometer (XRD) were employed to characterize the microstructure, elemental distribution and phase composition of the CaP coatings. Simulated body fluid (SBF) immersion test was used to evaluate the coating bioactivity and degradability. Systemic toxicity test was used to evaluate the coating biocompatibility. Fluoride ion selective electrode (ISE) was used to measure F(-) ions concentration during 30 days SBF immersion. The CaP coatings effectively reduced the corrosion rate and the surfaces of CaP coatings were covered by a new layer formed of numerous needle-like and scale-like apatites. The formation of these calcium phosphate apatites indicates that the coatings have excellent bioactivity. The coatings formed in (NaPO3)6-containging electrolyte exhibit thicker thickness, higher adhesive strength, slower degradation rate, better apatite-inducing ability and biocompatibility.

  6. Isolation and characterization of biogenic calcium carbonate/phosphate from oral bacteria and their adhesion studies on YSZ-coated titanium substrate for dental implant application

    Indian Academy of Sciences (India)

    GOBI SARAVANAN KALIARAJ; KAMALAN KIRUBAHARAN; G PRADHABAN; P KUPPUSAMI; VINITA VISHWAKARMA

    2016-04-01

    Biogenic calcium carbonate/phosphate were isolated and characterized from oral bacteria (CPOB). The crystalline nature and morphology of calcium carbonate/phosphate were characterized by X-ray diffraction (XRD)and field emission scanning electron microscopy (FESEM), respectively. XRD analysis revealed the cubic phase of YSZ coating as well as biogenic calcium carbonate (rhombohedral) and calcium phosphate oxide (hexagonal) wasobserved from CPOB. FESEM confirmed the extracellular synthesis of calcium compounds. Bacterial adhesion result reveals that YSZ coating drastically reduce bacterial invasion than titanium substrate.

  7. A biomimetic strategy to form calcium phosphate crystals on type I collagen substrate

    Energy Technology Data Exchange (ETDEWEB)

    Xu Zhang [Department of Restorative Dentistry, Faculty of Dentistry, National University of Singapore, 5 Lower Kent Ridge Road 119074, Singapore (Singapore); Neoh, Koon Gee [Department of Chemical and Biomolecular Engineering, National University of Singapore, Kent Ridge 119260, Singapore (Singapore); Kishen, Anil, E-mail: anil.kishen@utoronto.ca [Discipline of Endodontics, Faculty of Dentistry, University of Toronto, 124 Edward Street, Toronto, ON (Canada)

    2010-07-20

    Objective: The aim of this study is to induce mineralization of collagen by introducing phosphate groups onto type I collagen from eggshell membrane (ESM) by treating with sodium trimetaphosphate (STMP). This strategy is based on the hypothesis that phosphate groups introduced on collagen can mimic the nucleating role of phosphorylated non-collagenous proteins bound to collagen for inducing mineralization in natural hard tissue. Method: The collagen membrane was phosphorylated by treating it with a solution of STMP and saturated calcium hydroxide. The phosphorylated collagen was subsequently exposed to a mineralization solution and the pattern of mineralization on the surface of phosphorylated collagen substrate was analyzed. Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), field emission electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and microhardness test were used to characterize the collagen substrate and the pattern of minerals formed on the collagen surface. Results: The FTIR and EDX results indicated that the phosphate groups were incorporated onto the collagen surface by treatment with STMP. During the mineralization process, the plate-like mineral, octacalcium phosphate (OCP), which was initially formed on the surface of ESM, was later transformed into needle-like hydroxyapatite (HAP) as indicated by the SEM, FESEM, EDX and XRD findings. The microhardness test displayed significant increase in the Knoop hardness number of the mineralized collagen. Conclusions: Phosphate groups can be introduced onto type I collagen surface by treating it with STMP and such phosphorylated collagen can induce the mineralization of type I collagen.

  8. Characterization of chlorhexidine-releasing, fast-setting, brushite bone cements.

    Science.gov (United States)

    Young, Anne M; Ng, Poon Yun J; Gbureck, Uwe; Nazhat, Showan N; Barralet, Jake E; Hofmann, Michael P

    2008-07-01

    The effect of antibacterial chlorhexidine diacetate powder (CHX) on the setting kinetics of a brushite-forming beta-tricalcium phosphate/monocalcium phosphate monohydrate (beta-TCP/MCPM) cement was monitored using attenuated total reflection Fourier transform infrared spectroscopy. The final composition of the set cement with up to 12 wt.% CHX content before and after submersion in water for 24h, the kinetics of chlorhexidine release and the total sample mass change in water over four weeks was monitored using Raman mapping, UV spectroscopy and gravimetry, respectively. Below 9 wt.%, CHX content had no significant effect on brushite formation rate at 37 degrees C, but at 12 wt.% the half-life of the reaction decreased by one-third. Raman mapping confirmed that brushite was the main inorganic component of the set cements irrespective of CHX content, both before and after submersion in water. The CHX could be detected largely as discrete solid particles but could also be observed partially dispersed throughout the pores of the set cement. The percentage of CHX release was found to follow Fick's law of diffusion, being independent of its initial concentration, proportional to the square root of time and, with 1mm thick specimens, 60% was released at 24h. Total set cement mass loss rate was not significantly affected by CHX content. On average, cements exhibited a loss of 7 wt.% assigned largely to surface phosphate particle loss within the initial 8h followed by 0.36 wt.% per day.

  9. Chlorhexidine-calcium phosphate nanoparticles - Polymer mixer based wound healing cream and their applications.

    Science.gov (United States)

    Viswanathan, Kaliyaperumal; Monisha, P; Srinivasan, M; Swathi, D; Raman, M; Dhinakar Raj, G

    2016-10-01

    In this work, we developed a wound healing cream composed of two different polymers, namely chitosan and gelatin with chlorhexidine along with calcium phosphate nanoparticles. The physicochemical properties of the prepared cream were investigated based on SEM, EDX, Raman, FTIR and the results indicated that the cream contained gelatin, chitosan, calcium phosphate nanoparticles and chlorhexidine. The maximum swelling ratio studies indicated that the ratio was around of 52±2.2 at pH7.4 and the value was increased in acidic and alkaline pH. The antimicrobial activity was tested against bacteria and the results indicated that, both chlorhexidine and the hybrid cream devoid of chlorhexidine exhibited antimicrobial activity but the chlorhexidine impregnated cream showed three fold higher antimicrobial activity than without chlorhexidine. In vivo wound healing promoting activities of hybrid cream containing 0.4mg/L chlorhexidine were evaluated on surgically induced dermal wounds in mice. The results indicated that the cream with incorporated chlorhexidine significantly enhanced healing compared with the control samples. For the field validations, the veterinary clinical animals were treated with the cream and showed enhanced healing capacity. In conclusion, a simple and efficient method for design of a novel wound healing cream has been developed for veterinary applications.

  10. Microwave-Assisted Hydrothermal Rapid Synthesis of Calcium Phosphates: Structural Control and Application in Protein Adsorption

    Directory of Open Access Journals (Sweden)

    Zhu-Yun Cai

    2015-07-01

    Full Text Available Synthetic calcium phosphate (CaP-based materials have attracted much attention in the biomedical field. In this study, we have investigated the effect of pH values on CaP nanostructures prepared using a microwave-assisted hydrothermal method. The hierarchical nanosheet-assembled hydroxyapatite (HAP nanostructure was prepared under weak acidic conditions (pH 5, while the HAP nanorod was prepared under neutral (pH 7 and weak alkali (pH 9 condition. However, when the pH value increases to 11, a mixed product of HAP nanorod and tri-calcium phosphate nanoparticle was obtained. The results indicated that the pH value of the initial reaction solution played an important role in the phase and structure of the CaP. Furthermore, the protein adsorption and release performance of the as-prepared CaP nanostructures were investigated by using hemoglobin (Hb as a model protein. The sample that was prepared at pH = 11 and consisted of mixed morphologies of nanorods and nanoprisms showed a higher Hb protein adsorption capacity than the sample prepared at pH 5, which could be explained by its smaller size and dispersed structure. The results revealed the relatively high protein adsorption capacity of the as-prepared CaP nanostructures, which show promise for applications in various biomedical fields such as drug delivery and protein adsorption.

  11. A Study for Tooth Bleaching via Carbamide Peroxide-Loaded Hollow Calcium Phosphate Spheres

    Directory of Open Access Journals (Sweden)