高速逆流法分离纯化五味子中的五味子酚

Preparative separation of Schisanhenol from Schisandra chinensis by high-speed countercurrent chromatography

95%乙醇提取五味子种子的粗提物,经过硅胶分离后的1g粗品用高速逆流色谱首次分离得到122mg纯度为99.9%的五味子酚,结构经ESI-MS,MS/MS鉴定。同时分离得到86mg纯度为98%的五味子甲素、93mg纯度为97%的五味子乙素和114mg纯度为99%的五味子酯甲。两相溶剂系统确定为正已烷-甲醇-水(体积比为7∶6∶1)的三元溶剂系统,上相为固定相,下相为流动相,转速为800r/min,流速为2.0mL/min。

Following an initial purification step on silica gel, preparative high speed countercurrent chromatography （HSCCC） with a two-phase solvent system composed of n-hexane-methanol-water （volume fraction 7：6： 1 ） was used to isolate and separate first schisanhenol and then deoxyschisandrin, 7-Schisandrin and schisantherin A from Schisandra chinensis with the upper organic phase system as the stationary phase and the lower phase system as the mobile phase. Yields of 122 mg Schisanhenol, 86 nag deoxyschisandrin, 93 mg 7-Schisandrin, and 114 mg Schisantherin A were obtained.