巫山淫羊藿中朝藿定C的快速高效制备工艺优化

Optimized Rapid Preparation of Epimedin C from Epimedium wushanense T.S.Ying

建立了一种快速高效分离纯化巫山淫羊藿中朝藿定C的方法。以朝藿定C含量为指标,采用静态和动态吸附与解吸筛选大孔吸附树脂及最佳工艺条件,利用动态轴向压缩柱系统(DAC-HB50)完成精制。结果表明,巫山淫羊藿提取物经HPD-5000大孔树脂粗分离纯化后,朝藿定C纯度为55.27%,总收率为74%,再经采用DAC-HB50系统的制备色谱精制,朝藿定C纯度为98.91%,收率为80.36%。纯化产物的HPLC和核磁共振数据与朝藿定C对照品基本一致。本法通过两步即可实现巫山淫羊藿中朝藿定C的完全分离,操作简便、快速、高效和经济,为巫山淫羊藿中朝藿定C的高纯度规模化制备提供了新途径。

A fast and efficient method for the separation and purification of epimedin C from Epimedium wushanense T.S.Ying was established.The properties of epimedin C on sixteen kinds of macroporous resins were investigated by static adsorption/desorption and dynamic separation experiments to obtain the optimal macroporous resin and process conditions.The crude extraction of Epimedium wushanense T.S.Ying was separated with HPD-5000 macroporous resin,and epimedin C was obtained in a yield of 74%with a purity of 55.27%.Then,after purification by dynamic axial compression column(DAC-HB50)preparative HPLC system,the purity of epimedin C were further improved to 98.91%in a yield of 80.36%.The HPLC and NMR data of the purified product were basically consistent with those of the epimedin C reference substance.This method can realize the complete separation and purification of epimedin C from Epimedium wushanense T.S.Ying in two steps,and provide a new way for the high purity and largescale preparation of epimedin C.