高速逆流色谱法分离纯化黄芪中毛蕊异黄酮苷和芒柄花苷

目的:建立高速逆流色谱法(HSCCC)分离纯化黄芪中毛蕊异黄酮苷和芒柄花苷的方法。方法:黄芪粗提物分别采用正己烷-乙酸乙酯-甲醇-水(1∶10∶2∶10)、乙酸乙酯-乙醇-正丁醇-水(30∶10∶6∶50)两相溶剂系统进行HSCCC分离纯化,下相为流动相,流速分别为2.5 m L·min~(-1)、2.0 mL·min~(-1),转速900 r·min~(-1),检测波长254 nm,所得产物采用高效液相进行纯度测定。结果:300 mg黄芪粗提物分离得到毛蕊异黄酮苷(20 mg)、芒柄花苷(25 mg),两个化合物经高效液相色谱法(HPLC)分析,纯度均大于95%。结论:高速逆流色谱法是一种高效分离纯化黄芪中毛蕊异黄酮苷和芒柄花苷的方法。

Separation and Purification of Calycosin-7-glucoside and Ononin from Astragalus Membranceus by High-speed Counter-current Chromatography

Objective:To establish the method of separating and purifying the calycosin-7-glucoside and ononin from astragalus membranceus by high-speed counter-current chromatography.Methods:The crude extract of astragalus membranceus was separated and purified by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water(1∶10∶2∶10) and ethyl acetate-ethanol-n-butyl alcohol-water(30∶10∶6∶50) respectively.The lower phases were used as mobile phases with two flow rates of 2.5 mL·min~(-1) and 2.0 mL·min~(-1),while the apparatus rotated at 900 r·min~(-1) and the wavelength were detected at 254 nm.The structures of the target compounds were identified by HPLC.Results:From 300 mg crude extract of astragalus membranceus,two compounds with calycosin-7-glucoside(20 mg) and ononin(25 mg) were obtained.The purities of these two compounds determined by HPLC were both over 95%.Conclusion:High-speed counter-current chromatography is an efficient method for separating and purifying the calycosin-7-glucoside and ononin from astragalus membranceus.