微波辅助溶剂热法制备磷酸钙微球和多面体

doi:10.3724/SP.J.1077.2014.14148

摘要/Abstract

摘要：

磷酸钙材料具有良好的生物相容性, 被广泛应用于生物材料领域。本研究以Ca(CH₃COO)2、NaH₂PO₄?2H₂O和双亲嵌段共聚物PLA-mPEG为原料, 通过微波辅助120℃水热反应30 min, 合成了自组装结构磷酸钙微球。以相同的反应原料, 在水和乙二醇混合溶剂中, 通过微波辅助120℃溶剂热反应30 min, 制备了具有多面体结构的磷酸钙。通过X射线粉末衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)和热重分析(TG)对所制备样品的物相和形貌进行了表征。研究发现乙二醇的加入对磷酸钙的结构和形貌具有显著的影响。以牛血红蛋白为模型, 研究了所制备的两种不同磷酸钙材料的蛋白吸附效果。磷酸钙材料的牛血红蛋白吸附量随装载溶液中牛血红蛋白浓度的增加而增大, 随样品制备过程中的乙二醇加入量的增加而减小。

关键词: 生物材料, 磷酸钙, 微波, 自组装, 蛋白吸附

Abstract:

Synthetic calcium phosphate (CaP) has been investigated as promising biomaterial due to its excellent biocompatibility. CaP nanosheet-assembled microspheres were prepared using Ca(CH₃COO)₂, NaH₂PO₄•2H₂O and PLA-mPEG in aqueous solution by microwave-assisted hydrothermal method at 120℃ for 30 min. Meanwhile, CaP polyhedral were prepared using Ca(CH₃COO)₂, NaH₂PO₄•2H₂O and PLA-mPEG in mixed solvent of water and ethylene glycol (EG) by microwave-assisted solvothermal method at 120℃ for 30 min. The products were characterized with X-ray powder diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM) and thermogravimetric analysis (TG). EG showed a significant effect on the chemical composition and morphology of the product. The hemoglobin protein adsorption properties of the as-prepared products were investigated. The Hb adsorption amount increased with increasing Hb initial concentration, and were decreased with increasing volume of EG.

Key words: biomaterials, calcium phosphate, microwave, self-assembling, protein adsorption

中图分类号:

TQ174

陈峰, 孙团伟, 漆超, 吴进, 崔大祥, 朱英杰. 微波辅助溶剂热法制备磷酸钙微球和多面体[J]. 无机材料学报, 2014, 29(7): 776-780.

CHEN Feng, SUN Tuan-Wei, QI Chao, WU Jin, CUI Da-Xiang, ZHU Ying-Jie. Microwave-assisted Solvothermal Synthesis of Calcium Phosphate Microspheres and Polyhedra[J]. Journal of Inorganic Materials, 2014, 29(7): 776-780.

图/表 6

Fig. 1 SEM images of CaP products prepared using Ca (CH3COO)2, NaH2PO4•2H2O and PLA-mPEG in mixed solvent of water and EG by the microwave-assisted solvothermal method at 120℃ for 30 min The volume of EG: (a,b) 0 mL; (c,d) 10 mL; (e,f) 15 mL; (g,h) 20 mL

Fig. 2 TEM micrographs (a)-(d) of the CaP products prepared using Ca(CH3COO)2, NaH2PO4•2H2O and PLA-mPEG in mixed solvent of water and EG by the microwave-assisted solvothermal method at 120℃ for 30 min The volume of EG: (a) 0 mL; (b) 10 mL; (c) 15 mL; (d) 20 mL

Fig. 3 Schematic illustration of the formation process of the CaP microspheres and polyhedra by the microwave-assisted hydrothermal/solvothermal methods

Fig. 4 XRD patterns (a) and FTIR spectra (b) of the products prepared using Ca(CH3COO)2, NaH2PO4•2H2O and PLA-mPEG in mixed solvent of water and EG with different volumes of EG by the microwave-assisted solvothermal method at 120℃ for 30 min

Fig. 5 TG curves of the products prepared using Ca (CH3COO)2, NaH2PO4•2H2O and PLA-mPEG in mixed solvent of water and EG with different volumes of EG by the microwave-assisted solvothermal method at 120℃ for 30 min

Fig. 6 Hb protein adsorption properties of the products prepared using Ca(CH3COO)2, NaH2PO4•2H2O and PLA-mPEG in mixed solvent of water and EG with different volumes of EG by the microwave-assisted solvothermal method at 120℃ for 30 min

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