Properties Of Calcium Phosphate Cement Research Articles

Mechanical properties of calcium phosphate based dental filling and regeneration materials.

The objective of this study was to compare the mechanical properties of calcium phosphate cements (CPC) for possible dental applications with varied liquid and powder compositions under the same testing condition. Cements studied in this experiment were divided into two groups of CPC not containing polymer and polymeric CPC (PCPC). Cement powder was formed by combining equimolar amounts of dicalcium phosphate anhydrous and tetracalcium phosphate, or acrylic resin polymer powder mixture. The CPC specimens for the compressive strength (CS) and diametral tensile strength (DTS) measurements were prepared by mixing powder and liquid for 30 s with a powder/liquid ratio of 3:1, and subsequently packing the paste into a brass mould. The specimens were kept at 37 degrees C and 100% relative humidity for 24 h before measurements were conducted on a Universal Testing Machine with a cross-head speed of 1 mm min-1. The CS of CPC was 0.14-10.29 MPa and that of PCPC was 0.26-117.58 MPa. The DTS of CPC was 0.10-4.56 MPa and that of PCPC was 0.07-22.54 MPa. The CS and DTS were very diverse depending on the composition of powder and liquid. Some compositions showed higher values than commercial liners. Thus compositions of 2% carboxymethyl cellulose + 35% citric acid in phosphate buffered saline (PBS), 20% gelatin in PBS, 2% sodium alginate in PBS, 20-40% aqueous acrylic-maleic copolymer solution, and some of the HPMC and PMVE-Ma solutions exhibited promising formulae for dentine regenerating materials. Acrylic resin-PCPC group showed generally higher CS and DTS values. Based on this study, further studies on the reaction with odontoblast and resultant dentine regeneration should be performed using promising compositions.

The Effects of S-Chitosan on the Physical Properties of Calcium Phosphate Cements

Water-soluble disodium (1→4)-2-deoxy-2-sulfoamino-β-d-glucopyranuronan (S-chitosan) was prepared from chitin by successive N-deacetylation, specific carboxylation at C-6 and sulfonation. Its structure was characterized by IR spectra and elemental analysis. The S-chitosan was added to two easily developed calcium phosphate cements (CPCs). One cement was monocalcium phosphate monohydrate (MPCM) with calcium oxide (CaO) in a 1M phosphate buffer (pH 7.4)(CPC-I); the other cement was dicalcium phosphate dihydrate (DCPD) with calcium hydroxide [Ca(OH)2] in a 1M Na2HPO4 solution (CPC-II). In vitro experiments showed that when S-chitosan where added to the liquid phases that the resulting S-chitosan containing CPCs had higher mechanical strengths and slightly prolonged setting times. The polyanion enhanced the mechanical strength of the CPCs by increasing the dissolubility of the cement start materials and binding the calcium ions strongly afterwards. An excess of the polyanion destroys the balances of the formulations of CPCs and lead to very slow setting processes or no setting at all.

Transforming growth factor- β1 incorporation in an α-tricalcium phosphate/dicalcium phosphate dihydrate/tetracalcium phosphate monoxide cement: release characteristics and physicochemical properties

The osteoconductive properties of calcium phosphate cements (CPCs) may be improved by the addition of growth factors, such as recombinant human transforming growth factor- β1 (rhTGF- β1). Previously we have shown that rhTGF- β1 was released from cement enriched with rhTGF- β1 and subsequently stimulated the differentiation of pre-osteoblastic cells from adult rat long bones. It is unknown whether the addition of rhTGF- β1 changes the material properties of this α-tricalcium-phosphate ( α-TCP)/tetracalcium-phosphate-monoxide (TeCP)/dicalcium-phosphate-dihydrate (DCPD) cement, and what the characteristics of the release of rhTGF- β1 from this CPC are. Therefore, in the present study we determined the release of rhTGF- β1 from cement pellets in vitro. The possible intervening effects of the CPC modification for intermixing rhTGF- β1 on physicochemical properties were studied by assessing the compressive strength and setting time, as well as crystallinity, calcium to phosphorus ratio, porosity and microscopic structure. Most of the previously incorporated rhTGF- β1 in the cement pellets was released within the first 48 h. For all concentrations of rhTGF- β1 intermixed (100 ng–2.5 mg/g CPC), approximately 0.5% of the amount of rhTGF- β1 incorporated initially was released in the first 2 h, increasing to 1.0% after 48 h. The release of rhTGF- β1 continued hereafter at a rate of about 0.1% up to 1 week, after which no additional release was found. The initial setting time, nor the final setting time was changed in control cement without rhTGF- β1 (standard CPC) or in cement modified for rhTGF- β1 (modified CPC) at 20°C and 37°C. Setting times were more than six times decreased at 37°C compared to 20°C. The compressive strength was initially low for both standard CPC and modified CPC, after which it increased between 24 h and 8 weeks. The compressive strength for the modified CPC was significantly higher compared with standard at 1, 2, and 8 weeks after mixing. X-ray diffraction revealed that both standard and modified CPC changed similarly from the original components into crystalline apatite. The calcium to phosphorus ratio as determined by an electron microprobe did not differ at all time points measured for standard CPC and modified CPC. In both standard CPC and modified CPC the separated particles became connected by crystals, forming a structure in which the particles could hardly be recognised in a densifying matrix with some small pores. The present study shows that the calcium phosphate cement is not severely changed by modification for the addition of rhTGF- β1. The addition of rhTGF- β1 in CPC enhances the biologic response as shown in our previous study and did not interfere with the aimed physical and chemical properties as shown in this study. We conclude that the addition of rhTGF- β1 enlarges the potential of the CPC in bone replacement therapy.

Transforming growth factor-beta1 incorporation in a calcium phosphate bone cement: material properties and release characteristics.

The bone regenerative properties of calcium phosphate cements (CPCs) may be improved by the addition of growth factors, such as recombinant human transforming growth factor-beta1 (rhTGF-beta1). Previously, we showed that rhTGF-beta1 in CPC stimulated the differentiation of preosteoblastic cells from adult rat long bones. The intermixing of rhTGF-beta1 in CPC, which was subsequently applied to rat calvarial defects, enhanced bone growth around the cement and increased the degradation of the cement. However, it is unknown whether the addition of rhTGF-beta1 changes the material properties of CPC and what the characteristics of the release of rhTGF-beta1 from CPC are. Therefore, we determined in this study the release of rhTGF-beta1, in vitro, from the cement pellets as implanted in the rat calvariae. The possible intervening effects of rhTGF-beta1 intermixing on the clinical compliance of CPC were studied through an assessment of its compressive strength and setting time, as well as its crystallinity, calcium-to-phosphorus ratio, porosity, and microscopic structure. We prepared CPC by mixing calcium phosphate powder (58% alpha-tricalcium phosphate, 25% anhydrous dicalcium phosphate, 8.5% calcium carbonate, and 8.5% hydroxyapatite) with a liquid (3 g/mL). The liquid for standard CPC consisted of water with 4% disodium hydrogen phosphate, whereas the liquid for modified CPC was mixed with an equal amount of 4 mM hydrochloride with 0.2% bovine serum albumin. The hydrochloride liquid contained rhTGF-beta1 in different concentrations for the release experiments. Most of the rhTGF-beta1 incorporated in the cement pellets was released within the first 48 h. For all concentrations of intermixed rhTGF-beta1 (100 ng to 2.5 mg/g of CPC), approximately 0.5% was released in the first 4 h, increasing to 1.0% after 48 h. Further release was only about 0.1% from 2 days to 8 weeks. CPC modification slightly increased the initial setting time at 20 degrees C from 2.6 to 5 min but had no effect on the final setting time of CPC at 20 degrees C or the initial and final setting times at 37 degrees C. The compressive strength was increased from 18 MPa in the standard CPC to 28 MPa in the modified CPC only 4 h after mixing. The compressive strength diminished in the modified CPC between 24 h and 8 weeks from 55 to 25 MPa. No other significant change was found with the CPC modification for rhTGF-beta1. X-ray diffraction revealed that standard and modified CPCs changed similarly from the original components, alpha-tricalcium phosphate and anhydrous dicalcium phosphate, into an apatite cement. The calcium-to-phosphorus ratio, as determined with an electron microprobe, did not differ for standard CPC and modified CPC. Standard and modified CPCs became dense and homogeneous structures after 24 h, but the modified CPC contained more crystal plaques than the standard CPC, as observed with scanning electron microscopy (SEM). SEM and back- scattered electron images revealed that after 8 weeks the cements showed equally and uniformly dense structures with microscopic pores (<1 microm). Both CPCs showed fewer crystal plaques at 8 weeks than at 24 h. This study shows that CPC is not severely changed by its modification for rhTGF-beta1. The prolonged setting time of modified cement may affect the clinical handling but is still within acceptable limits. The compressive strength for both standard and modified cements was within the range of thin trabecular bone; therefore, both CPCs can withstand equal mechanical loading. The faster diminishing compressive strength of modified cement from 24 h to 8 weeks likely results in early breakdown and so might be favorable for bone regeneration. Together with the beneficial effects on bone regeneration from the addition of rhTGF-beta1 to CPC, as shown in our previous studies, we conclude that the envisaged applications for CPC in bone defects are upgraded by the intermixing of rhTGF-beta1. Therefore, the combination of CPC and rhTGF-beta1 forms a promising synthetic bone graft.

Solution property of calcium phosphate cement hardening body

In this paper, the solution property of calcium phosphate cement (CPC) hardening bodies with various ratios of calcium to phosphate were studied. The solution property included solubility and behavior in simulated blood phosphoric acid solutions with selected initial concentrations at 37°C. When the ratios of calcium to phosphate were 1.67, 1.60, 1.55, 1.50, the solubility products, −log K sp, were 99.2–102, 94.7–94.8, 89.6–90.5, 85.5–86.4, respectively. All these were significantly bigger than the values reported by the references due to the low crystallinity and calcium deficiency in the calcium phosphate cement hardening body. When CPC with Ca/P = 1.50 was immersed in fixed volumes of simulated blood plasma, both the calcium and phosphate concentrations in the solution increased, while for the samples with a ratio of 1.67, the concentrations decreased. These results showed that the simulated blood plasma was supersaturated when Ca/P = 1.67 but unsaturated Ca/P = 1.50. It was deduced that when CPC was implanted in the bodies, the specimen with the ratio of 1.5 was degraded faster than with the sample of 1.67.

Production and characterization of new calcium phosphate bone cements in the CaHPO4-alpha-Ca3(PO4)2 system: pH, workability and setting times.

The initial setting properties of calcium phosphate cements in the CaHPO4-alpha-Ca3(PO4)2 (DCP-alpha-TCP) system have been investigated. Interest was focused on the pH, workability, cohesion time and initial and final setting times. The addition of CaCO3 modified the structure of the cement reaction product such that it became more similar to the apatite phase in bone mineral. The addition of 10% w/w of CaCO3 reduced the viscosity of the cement pastes resulting in an increase in initial and final setting times and improved injectability.

Improvement of the mechanical properties of new calcium phosphate bone cements in the CaHPO4-alpha-Ca3(PO4)2 system: compressive strength and microstructural development.

The hardening properties of calcium phosphate cements in the CaHPO4-alpha-Ca3(PO4)2 (DCP-alpha-TCP) system have been investigated with interest focused on the compressive strength and microstructure development. Previous studies have shown that the addition of CaCO3(CC) leads to a modification of the calcium-deficient apatite structure of the reaction product, which results in a material more similar to the apatite in bone mineral. The addition of 10% w/w of CC to the initial DCP-alpha-TCP powder mixture resulted, with time, in a retardation of the development of compressive strength. However, the optimum compressive strength reached values up to 40% higher than CC-free samples. This retarding effect also has been monitored as a function of the calcium to phosphorus (Ca/P) ratio of the DCP and alpha-TCP mixture, showing the importance of the final cement properties of the relative quantities of the reactants in the mixture.

Basic properties of calcium phosphate cement containing atelocollagen in its liquid or powder phases

The basic properties of calcium phosphate cement (CPC) containing atelocollagen, the main component of the organic substrate in bone, were studied in an initial evaluation for the fabrication of modified CPC. The setting time of conventional CPC (c-CPC) was prolonged to over 100 min when c-CPC contained 1% or more atelocollagen. The diametral tensile strength (DTS) of c-CPC decreased linearly with the collagen content, descending to below the detection limit when the c-CPC contained 3% or more atelocollagen. Therefore, use of c-CPC as the base cement seems inappropriate for the fabrication of atelocollagen-containing CPC. In contrast, the cement set at 9–34 min when fast-setting CPC (FSCPC) was used as the base cement and contained 1–5% atelocollagen, respectively. Although addition of atelocollagen resulted in the decrease of DTS of the set mass, the DTS was approximately the same, 6–8 MPa, at contents of atelocollagen between 1% and 5%. When atelocollagen was added to FSCPC, the handling property was improved significantly. The paste also became more adhesive with increase in atelocollagen content. These properties are desirable for its use in surgical procedures since, for example, bony defects can be filled easily and without a space interposed between the bone and cement paste. Although there are some disadvantages for the addition of atelocollagen to CPC, it can be accepted as long as FSCPC was used as the base cement. We conclude that further evaluations of the effects of atelocollagen, such as biocompatibility, bone synthesis, and bone replacement behaviour should be done, using FSCPC as the base cement.

Effects of hydroxypropyl methylcellulose and other gelling agents on the handling properties of calcium phosphate cement

The calcium phosphate cement (CPC) used in this study was formed by combining equimolar amounts of tetracalcium phosphate (TTCP) and dicalcium phosphate anhydrous (DCPA). This powder, when mixed with water, sets to a hard cement in about 30 min. However, the water-based CPC paste is not highly cohesive and is vulnerable to washout until hardening occurs. The objectives of this study were to investigate the effects on handling properties, washout resistance, cement hardening behavior, and mechanical properties of adding several gelling agents to CPC paste. Aqueous solutions that contained a mass fraction of 2–4% of hydroxypropyl methylcellulose (HPMC), carboxyl methyl-cellulose (CMC), chitosan acetate, and chitosan lactate were used as cement liquids. Hardening time was measured by the Gilmore needle test; resistance to washout was evaluated by the disintegration of the cement specimen in water with agitation; and mechanical strength was evaluated by the measurement of diametral tensile strength and compressive strength. Handling properties were greatly improved by the addition of HPMC, CMC, chitosan acetate, and chitosan lactate. Hardening time was retarded by the additions of HPMC and CMC, and mechanical strength was weakened by the addition of either the chitosan lactate or the chitosan acetate. © 1997 John Wiley & Sons, Inc. J. Biomed Mater Res, 35, 273–277, 1997.