微粉化反式肉桂酸的反溶剂重结晶法制备与表征  

Preparation and characterization of micronized trans-cinnamic acid by anti-solvent crystallization method

作　　者：赵修华[1] 刘影[1] 王卫国[1] 李娜[1] 葛云龙[1] 李永[1] 祖元刚[1] 

机构地区：[1]东北林业大学森林植物生态学教育部重点实验室,黑龙江哈尔滨150040

出　　处：《中草药》2014年第15期2165-2171,共7页Chinese Traditional and Herbal Drugs

基　　金：国家科技支撑计划课题(2012BAD21B05)

摘　　要：目的以乙醇做溶剂,超纯水作为反溶剂,HPMC作为表面活性剂制备反式肉桂酸(TCA)微粉,通过单因素分析法,对TCA微粉颗粒大小和形貌的主要影响因子(沉积时间、药物质量浓度、溶剂与反溶剂比、表面活性剂用量、搅拌强度)进行考察。方法分别利用透射电镜(TEM)、激光粒度分析方法、傅里叶变换红外光谱(FTIR)、质谱分析(LC-MS)、X射线衍射(XRD)、差示扫描(DSC)、溶出度对所得TCA微粉进行了表征。结果获得的TCA纳米粒为球形,平均粒径为130 nm;纳米化后的TCA质量分数由99.0%提高至99.8%,溶出速率是原药的1.67倍。结论采用反溶剂重结晶法制备TCA超微粉,能够提高TCA在水中的溶解度和分散性,为进一步的制剂开发提供基础。Objective Using ethanol as solvent, deionized water as anti-solvent, and HPMC as the surfactant, to prepare trans-cinnamic acid（TCA） micro powder by single factor analysis. The effects of five experimental parameters on the mean particle size（MPS） and morphology of TCA nanosuspension were investigated. Methods Transmission electron microscope（TEM）, laser granulometric analysis, Fourier transform infrared spectroscopy（FTIR）, high performance liquid chromatography-mass spectrometry（LC-MS）, X-ray diffraction（XRD）, differential scanning calorimetry（DSC）, and dissolution were used to analyze the characteristic of micronized TCA nanosuspension. Results The micronized TCA with an MPS of 130 nm was obtained under the optimum conditions. The dissolution rate of TCA nanosuspension was 1.67 times of raw drug. Conclusion Using anti-solvent recrystallization to prepare micronized TCA can improve the solubility and dispersion of TCA nanosuspension in water, and they provide the basis for further formulation development.

关 键 词：反溶剂法 反式肉桂酸 单因素分析法 超微粉 溶出度 抗氧化 生物利用度 

分 类 号：R283.6[医药卫生—中药学]