Masayuki Kon

Non-decay type fast-setting calcium phosphate cement: composite with sodium alginate.

Non-decay type fast-setting calcium phosphate cement (nd-FSCPC) was prepared by introducing sodium alginate (0-2.0 wt%) into the liquid phase of FSCPC. nd-FSCPC was stable even when the cement paste was immersed in distilled water immediately after mixing, whereas conventional FSCPC (c-FSCPC) decayed completely within 1 min upon immersion. The setting time of the cement, approximately 5 min, was not dependent on the presence of sodium alginate. In contrast, the introduction of sodium alginate into conventional CPC, i.e. CPC without neutral phosphate in the liquid phase, resulted in no setting when the amount of sodium alginate introduced was more than 1 wt%. Powder X-ray diffraction analysis revealed no significant difference for the conversion of cement to apatite for any concentrations of sodium alginate studied (0-2.0 wt%). The mechanical strength of the cement increased rapidly with the addition of sodium alginate up to 0.8 wt% when the cement paste was immersed and kept in distilled water at 37 degrees C, whereas further addition of sodium alginate decreased the mechanical strength. The results obtained in this investigation, taken together with sodium alginates known excellent biocompatibility and absorption behaviour, indicate that the use of sodium alginate composite FSCPC as nd-FSCPC should be of value in orthodontics and oral and maxillofacial surgery where the cement is exposed to blood.

In vivo setting behaviour of fast-setting calcium phosphate cement

The in vivo setting behaviour of fast-setting calcium phosphate cement (FSCPC) between femoral muscles of the rat was investigated to evaluate the possible value of FSCPC for medical and dental application. Conventional CPC (c-CPC) and FSCPC were implanted between femoral muscles, and various aspects of the setting behaviour such as setting time, mechanical strength and conversion ratio of cement into hydroxyapatite (HAP: Ca10(PO4)6(OH)2) were measured by the Vicat needle method, diametral tensile strength (DTS) measurement, and quantitative powder X-ray diffraction (XRD) analysis, respectively. The setting time of FSCPC in vivo was 5-7 min, in contrast to 48 min for c-CPC. As a result of its fast setting, set specimens of FSCPC showed higher mechanical strength from the initial stage than c-CPC. Higher DTS values were observed in FSCPC than c-CPC implanted after 24 h. Powder XRD analysis revealed faster conversion of FSCPC than c-CPC into HAP, which was responsible both for the faster setting and higher mechanical strength from the initial stage. We concluded, therefore, that FSCPC may be used for a wide range of clinical applications, i.e. fields where fast setting is required such as orthopaedic, plastic and reconstructive, and oral and maxillofacial surgery.

Non-decay type fast-setting calcium phosphate cement: Hydroxyapatite putty containing an increased amount of sodium alginate

A hydroxyapatite [(HAP) Ca10(PO4)6(OH)2] putty that behaves like a putty or self-curing resin was made by increasing the amount of sodium alginate in non-decay type fast-setting calcium phosphate cement (nd-FSCPC). nd-FSCPC became viscous as the sodium alginate concentration was increased. The best handling properties were obtained when nd-FSCPC contained 8% sodium alginate in its liquid phase. When a 2-kg glass plate was placed on the paste, HAP putty spread to form an area three times that of FSCPC paste. Thus, HAP putty is expected to be easier to use than FSCPC in the filling of bone defects. HAP putty did not decay; in fact, it set within approximately 20 min when immersed in distilled water immediately after mixing. The wet diametral tensile strength value of HAP putty was approximately 12 MPa after 24 h, the same as that for nd-FSCPC containing 0.5% sodium alginate in its liquid phase, or FSCPC that is free from sodium alginate. The elements constituting set HAP putty were examined using powder X-ray diffraction and found to be predominantly apatitic minerals after 24 h. Since the handling properties of a putty or self-curing resin-like cement are very useful in certain surgical procedures, HAP putty made by increasing the sodium alginate concentration in nd-FSCPC is potentially a valuable new biomaterial for use in plastic and reconstructive surgery, as well as oral and maxillofacial surgery.

Effects of added antibiotics on the basic properties of anti-washout-type fast-setting calcium phosphate cement.

The effect of added antibiotics on the basic properties of anti-washout-type fast-setting calcium phosphate cement (aw-FSCPC) was investigated in a preliminary evaluation of aw-FSCPC containing drugs. Flomoxef sodium was employed as the antibiotic and was incorporated into the powder-phase aw-FSCPC at up to 10%. The setting time, consistency, wet diametral tensile strength (DTS) value, and porosity were measured for aw-FSCPC containing various amounts of flomoxef sodium. X-ray diffraction (XRD) analysis was also conducted for the identification of products. To evaluate the drug-release profile, set aw-FSCPC was immersed in saline and the released flomoxef sodium was determined at regular intervals. The spread area of the cement paste as an index of consistency of the cement increased progressively with the addition of flomoxef sodium, and it doubled when the aw-FSCPC contained 8% flomoxef sodium. In contrast, the wet DTS value decreased with increase in flomoxef sodium content. Bulk density measurement and scanning electron microscopic observation revealed that the set mass was more porous with the amount of flomoxef sodium contained in the aw-FSCPC. The XRD analysis revealed that formation of hydroxyapatite (HAP) from aw-FSCPC was reduced even after 24 h, when the aw-FSCPC contained flomoxef sodium at > or = 6%. Therefore, the decrease of wet DTS value was thought to be partly the result of the increased porosity and inhibition of HAP formation in aw-FSCPC containing large amounts of flomoxef sodium. The flomoxef sodium release from aw-FSCPC showed the typical profile observed in a skeleton-type drug delivery system (DDS). The rate of drug release from aw-FSCPC can be controlled by changing the concentration of sodium alginate. Although flomoxef sodium addition has certain disadvantageous effects on the basic properties of aw-FSCPC, we conclude that aw-FSCPC is a good candidate for potential use as a DDS carrier that may be useful in surgical operations.

Tissue response to fast-setting calcium phosphate cement in bone

Fast-setting calcium phosphate cement (FSCPC) is a promising new bioactive cement with a significantly short setting time (approximately 5-6 min) compared to conventional calcium phosphate cement (c-CPC) (30-60 min) at physiologic temperatures. As a result of its ability to set quickly, it is applicable in surgical procedures where fast setting is required. In this study, FSCPC was implanted in rat tibiae to evaluate tissue response and biocompatibility. FSCPC was converted to hydroxyapatite (HAP) in bone faster than c-CPC in the first 6 h. By 24 h, significant amounts of both FSCPC and c-CPC had been converted to HAP. The conversion of FSCPC into HAP further proceeded gradually, reaching 100% within 8 weeks. Infrared spectroscopic analysis disclosed the deposition of B-type carbonate apatite, which is a biological apatite contained in human dentin or bone, on the surface of the FSCPC. Histologically, FSCPC showed a tissue response similar to that of c-CPC. A slight inflammatory reaction was observed in the soft tissue apposed to both cements in the early period, and new bone was formed along the surface of the FSCPC at the adjacent bone. However, no resorption of either cement by osteoclasts or macrophages was observed within 8 weeks. We conclude that FSCPC is superior to c-CPC in clinical applications in oral and maxillofacial, orthopedic, plastic, and reconstructive surgery, since it shows a faster setting time and higher mechanical strength in the early period that are required in these surgical procedures, as well as osteoconductivity and excellent biocompatibility similar to that of c-CPC.

AMOUNT OF HYDROXYL RADICAL ON CALCIUM-ION-IMPLANTED TITANIUM AND POINT OF ZERO CHARGE OF CONSTITUENT OXIDE OF THE SURFACE-MODIFIED LAYER

To compare the surface properties of calcium-ion (Ca2+)-implanted titanium with those of titanium and to investigate the mechanism of bone conductivity of Ca2+-implanted titanium, amounts of hydroxyl radical of Ca2+-implanted titanium and titanium were estimated. Also, the point of zero charge (p.z.c.) of oxide constituting surface oxides of Ca2+-implanted titanium and titanium was determined. Results showed that the amount of active hydroxyl radical on Ca2+-implanted titanium was found to be significantly larger than that on titanium, indicating that the number of electric-charging sites of Ca2+-implanted titanium in electrolyte is more than that of titanium. The p.z.c. values of rutile (TiO2), anatase (TiO2), and perovskite (CaTiO3), were estimated to be 4.6, 5.9, and 8.1, respectively. Thus, Ca2+-implanted titanium surface is charged more positively in bioliquid than titanium, accelerating the adsorption of phosphate ions.

Non-decay type fast-setting calcium phosphate cement : setting behaviour in calf serum and its tissue response

Non-decay type fast-setting calcium phosphate cement (nd-FSCPC) was evaluated in terms of its setting behaviour in calf serum and its tissue response to investigate the feasibility of its clinical use in surgical applications. Non-decay type cements were prepared by adding various amounts of sodium alginate to the liquid phase of base cements, fast-setting calcium phosphate cement (FSCPC) and conventional calcium phosphate cement (c-CPC). Cement pastes were immersed in serum at 37 degrees C immediately after mixing, and decay behaviour, setting time and mechanical strength were measured to evaluate the possibility of their use in surgical applications. Also, nd-FSCPC was implanted into rat subcutaneous tissue for the initial evaluation of biocompatibility of this potential bioactive cement. nd-FSCPC set in approximately 6-7 min in serum, even when the cement paste was immersed in the serum immediately after mixing, whereas c-CPC and FSCPC decayed completely upon immersion. nd-FSCPC transforms to hydroxyapatite (HA) within 24 h and shows a diametral tensile strength of approximately 4-5 MPa. As a result of transformation to HA, nd-FSCPC showed excellent tissue response when implanted subcutaneously in rats. We conclude that nd-FSCPC has good potential value for use in orthopaedics, plastic and reconstructive surgery, and oral and maxillofacial surgery, where the cement is exposed to blood.

Non-decay type fast-setting calcium phosphate cement using chitosan

A non-decay type fast-setting calcium phosphate cement (nd-FSCPC) has been described, which did not decay but set within approximately 5–6 min even when the paste was immersed in serum immediately after mixing, and which forms hydroxyapatite as its end product. nd-FSCPC was produced by adding sodium alginate to the liquid phase of the base cement FSCPC. Sodium alginate forms a water-insoluble gel, and reduces the process of fluid penetration into the paste which is the cause of decay. The aim of this investigation was to confirm the mechanism of the non-decaying behaviour of nd-FSCPC proposed in a previous paper, using another chemical with properties similar to those of sodium alginate. Also, it was intended to further improve both the mechanical properties and tissue response of nd-FSCPC. Chitosan, which also forms a water-insoluble gel in the presence of calcium ions and has been reported to have pharmacologically beneficial effects on osteoconductivity, was added to the liquid phase of the base cement FSCPC. The cement thus prepared showed behaviour similar to that of nd-FSCPC using sodium alginate. The cement paste did not decay but set within approximately 5–6 min even when immersed in serum immediately after mixing. DTS value of the set mass was approximately 3–4 MPa, slightly lower than that of nd-FSCPC using sodium alginate, and no inhibitory effect was observed for the transformation of cement component to apatite within the range used in this investigation (up to 1.5%). Therefore, it was concluded that the mechanism of non-decaying behaviour was, at least in part, reduction of fluid penetration into the cement paste. nd-FSCPC using chitosan showed slightly poorer mechanical properties than that using sodium alginate. However, pharmacological effects such as osteoconductivity could be expected in nd-FSCPC using chitosan. Thus, this cement may be useful as a more sophisticated bioactive cement than nd-FSCPC using sodium alginate.

Strengthening of glass-ionomer cement by compounding short fibres with CaO-P2O5-SiO2-Al2O3 glass

The purpose of this study was to determine if short fibres of CaO-P2O5-SiO2-Al2O3 (CPSA) glass possessing a particular aspect ratio (length/diameter) could be used as a reinforcing agent for glass-ionomer cement. The powder of a commercial glass-ionomer cement (not resin modified) was mixed with variously sized CPSA glass short fibres before mixing with the liquid of the glass-ionomer cement. The mixed powders containing 60 mass% CPSA glass short fibres (diameter, 9.7 +/- 2.1 microm, aspect ratio, 5.0 +/- 0.9) obtained maximum values of 18 and 35 MPa for the diametral tensile strength (DTS) and flexural strength (FS) of set cements, respectively, after 24 h. These DTS and FS values were 1.8 and 4.5 times larger, respectively, than those of the set glass-ionomer cement not containing short fibres. Moreover, it was found that the addition of CPSA glass short fibres was remarkably more effective in the strengthening than electric glass (a typical glass fibre) short fibres. The results suggested that the CPSA glass short fibres acted as a reinforcing agent for strengthening the glass-ionomer cement, because of the shape of short fibres and reactivity between the mixing liquid and short fibres.

Development of calcium phosphate based functional gradient bioceramics

A functional gradient bioceramic that can function gradually with respect to body tissue was studied by changing the composition of calcium phosphate gradually from the surface to the inside. Diamond powder was spread on the surface of compact hydroxyapatite (HA) powder and fired at 1280 degrees C under reduced pressure, followed by firing under atmospheric conditions. The sintered body thus prepared was dense and alpha-tricalcium phosphate (alpha-TCP: alpha-Ca3(PO4)2) was found on its surface. The content of alpha-TCP gradually decreased with increasing depth from the surface. In contrast, the content of HA increased with increasing depth from the surface. The gradient ratio of alpha-TCP and HA depends on the firing time for each condition, i.e. reduced or atmospheric pressure. The alpha-TCP formation was ascribed to the decomposition of HA due to the spontaneous combustion of diamond powder.