一种高纯医用硫酸钙的制备及其生物相容性研究

Preparation and property research of a kind of high purity calcium sulfate

目的制备一种高纯医用硫酸钙(CaSO_4)并分析其生物相容性。方法尝试通过化学试剂反应合成的方法辅以多级洁净工艺,实现高纯度植入级CaSO_4材料的合成,用X射线衍射仪技术(XRD)进行晶相分析,热重-差热(TG/DTA)分析材料热转化温度,扫描电子显微镜(SEM)观察材料晶体形态,用电感耦合等离子体发射光谱仪(ICP-OES)检测所得材料的成分纯度和重金属元素含量,用体内异常毒性检测以判定材料是否符合安全性规定。结果 XRD结果显示所得材料为CaSO_4·2H_2O;该材料在150℃会失去结晶水;SEM显示CaSO_4·2H_2O形貌以棒状结构为主,宽度为7.5~10.0 um,无明显的团聚现象;ICP-OES测定其纯度为99.9%,未检测到重金属元素铅、汞、砷、镉,铁元素的含量为5.281 ppm;体内植入显示术后48 h内小鼠精神状态和进食等活动如常。结论本实验通过化学合成的方法辅以多级净化工艺制备CaSO_4,其纯度达到植入级硫酸钙规定,异常毒性检验符合生物相容性要求,可以进行后续植入硫酸钙的组织工程材料研究。

Objective To prepare a calcium sulfate material with high purity used in bone repair medicine. Methods A kind of high purity calcium sulfate material was prepared by precipitation with multi-stage clean iechnology. The chemical and structural components of the sample were characterized by means of X-Ray Diffraction （XRD） crystallography analysis. SEM was used to analyze the morphology of the sample. The decomposition temperature of the sample was tested by TG/DTG. The elemental analysis was conducted by ICP-OES. And the abnormal toxicity was tested to determine whether the materials complied with safety regulations. Results The result of XRD showed that the obtained sample was CaSO4·2H2O. [t lose crystal water and turned to CaSO4 at 150 ℃. Microstructure analysis by SEM indicated that the sample particles were rod with the width were 7.5-10.0 um and there were no agglomerating. No heavy metals such as Ph, Hg, AS, Cd, were detected and the content of iron was 5.281 ppm. The purity of CaSO4·2H2O was 99.9% which was calculated by ICP-OES. In vivo experiments showed the material had no abnormal cytotoxicity. Conclusion This kind of high purity calcium sulfate material prepared by precipitation with multi-stage clean technology with a capacity can meet the requirements of implant calcium sulfate materials and can he used for further tissue engineering scaffold research.