采用高速逆流色谱(HSCCC)方法从常春油麻藤豆荚中分离制备丁香脂素。HSCCC的溶剂系统条件为V(甲基叔丁基醚)∶V(甲醇)∶V(水)=2∶1∶1。从5 g粗提物中可一次分离得到纯度89.5%的丁香脂素单体1.28g,进一步重结晶可得到纯度98.1%的丁香脂素。分离得到的丁香脂素结构经电喷雾质谱(ESI-MS)以及核磁共振氢谱(1H NMR)和碳谱(13C NMR)进行鉴定。杭州不同地区的常春油麻藤豆荚中丁香脂素的含量在3.0 g/kg以上,是一种优质的天然丁香脂素资源,通过高速逆流色谱分离制备可获得大量天然丁香脂素。

The present study describes the separation of syringaresinol from the legume of Mucuna sempcrvircns by high-speed countercurrent chromatography(HSCCC) with a solvent system of methyl tert-butyl ether-methanol-water(2∶ 1∶ 1,v/v/v).Crude syringaresinol of 1.28 g with a purity of 89.5% was obtained from a separation of 5 g crude extracts.The crude syringaresinol was re-crystallized to more than 98% purity of syringaresinol.The chemical structure of the substance was identified by ESI-MS,1H NMR and 13C NMR.The syringaresinol content in the legume samples collected in different districts in Hangzhou were all more than 3.0 g/kg.This shows that the legume is an excellent resource for preparation of natural syringaresino which can be used for research and development of health food and medicine.