反溶剂重结晶法制备牡荆苷微粉工艺及其表征  

Preparation and Characterization of Micronized Vitexin by Antisolvent Recrystallization Method

作　　者：李旺[1,2,3] 王秋雪[1,2,3] 顾成波[1,2,3] 祖元刚[1,2,3] 赵修华[1,2,3] 付丽楠[1,2,3] 郭东杰[1,2,3] 

机构地区：[1]生物资源生态利用国家地方联合工程实验室,哈尔滨150040 [2]东北林业大学森林植物生态学教育部重点实验室,哈尔滨150040 [3]东北林业大学林业生物制剂教育部工程研究中心,哈尔滨150040

出　　处：《植物研究》2013年第1期104-108,共5页Bulletin of Botanical Research

基　　金：公益性行业科研专项经费项目(201204601);哈尔滨市科技创新人才专项资金(2011RFQXS074);中央高校基本科研业务费专项资金资助(DL09BA20)

摘　　要：为了提高牡荆苷溶出度,本实验采用反溶剂重结晶法(以N-甲基吡咯烷酮为溶剂,水为反溶剂)对牡荆苷原粉进行超细化研究。考察了药物浓度、溶剂与反溶剂体积比、搅拌转速及表面活性剂(PVP、Tween80、SDS)对牡荆苷微粉粒径的影响,确定牡荆苷微粉的最佳制备条件为:药液浓度为30 mg·mL-1,反溶剂与溶剂体积比为15∶1,搅拌转速为1 500 r·min-1,反溶剂中表面活性剂PVP浓度为8 mg·mL-1,上述条件下制备的牡荆苷微粉平均粒径为291.1 nm;采用扫描电镜(SEM)、X射线衍射(XRD)、差示扫描(DSC)、红外光谱(FTIR)对牡荆苷原粉与微粉进行了表征,与原粉相比牡荆苷微粉粒径变小,结晶度降低,其化学性质未发生改变,体外溶出度显著提高。To improve the dissolution rate of vitexin,the micronization of vitexin in an antisolvent recrystallization process using N-methylpyrrolidone（NMP） as solvent and water as antisolvent was studied in this paper.The effects of operating parameters including concentrations of vitexin solution,system temperatures,stirring rates and kinds of surfactants（PVP,Tween80,SDS） on the particle size of micronized vitexin were investigated.Particles of micronized vitexin with a mean particle size of 291.1 nm were obtained under the optimized process conditions（vitexin solution concentration 20 mg·mL-1,volume ratio of antisolvent to solvent 10∶ 1,stirring rate 1 500 r·min-1 and concentration of PVP 8 mg·mL-1）.The processed vitexin particles and the unprocessed one were characterized by scanning electron microscopy（SEM）,X-ray diffraction（XRD）,differential scanning calorimetry（DSC）,Fourier-transform infrared spectroscopy（FT-IR）.The results showed that antisolvent recrystallization process did not induce degradation of vitexin and the micronized vitexin had lower crystallinity.The chemical properties of the processed vitexin did not change when compared with the original drug,and there was a significant increase of the dissolution rate of the processed vitexin comparing with the unprocessed vitexin.

关 键 词：牡荆苷 反溶剂重结晶 微粉化 溶出度 

分 类 号：S567.1[农业科学—中草药栽培]