高速逆流色谱分离纯化防风中升麻素苷和5-O-甲基维斯阿米醇苷

Separation and Purification of Prim-O-glucosylcimifugin and 5-O-methylvisammioside from Saposhnikovia Divaricata by High-speed Counter-current Chromatography

建立了高速逆流色谱分离制备防风中有效成分升麻素苷和5-O-甲基维斯阿米醇苷的方法。防风根的粉末经甲醇浸泡提取和减压蒸馏,得粗提浸膏。以V(乙酸乙酯)∶V(正丁醇)∶V(水)=2∶7∶9为溶剂,上相为固定相,下相为流动相,流速2.0mL/min。从316mg防风粗提物中一步分离得到13.9mg升麻素苷和25mg5-O-甲基维斯阿米醇苷,纯度分别为98.1%和99.2%。采用ESI-MS,1H NMR和13C NMR对目标化合物的结构进行了鉴定。

High-speed counter-current chromatographic （HSCCC） method was successfully used to separate and purify prim-O-glucosyleimifugin and 5-O-methylvisammioside from Saposhnikovia divaricata（Thicz. ） Schischk , a traditional Chinese herb, with a solvent system composed of ethyl acetate-n-butanol-water （2 ： 7 ： 9, V/V）. The lower phase of the system was used as the mobile phase at the flow rate of 2.0 mL/min, and the upper phase was used as the stationary phase. The separation produced a total 13.9 mg prim-O-glucosyleimifugin and 25.0 mg 5-O-methylvisammioside with the purity of 98.1% and 99.2% determined by high performance liquid chromatography（HPLC） from 316 mg of crude sample from S. divaricata. The structures of isolated compounds were identified by ESI-MS, ^1H NMR and 13C NMR.