MPLC合p-HPLC法分离制备泽泻中23-乙酰泽泻醇B

Isolation and Preparation of Alisol B 23-acetate from Rhizoma Alismatis by MPLC Combined with p-HPLC

目的建立快速制备泽泻药材中23-乙酰泽泻醇B对照品的方法。方法采用中低压正相硅胶柱色谱(MPLC)合高压反相色谱法(p-HPLC),MPLC:硅胶柱:3 cm×13 cm,40 g;流动相:石油醚-乙酸乙酯梯度洗脱;流速:50 ml/min;p-HPLC:Ultimate XB-C18:21.2 mm×250 mm,10μm;流动相:乙腈-水(65:35);流速:15 mL/min;检测波长:208 nm。结果 MPLC合p-HPLC法一次可以从2 g泽泻乙酸乙酯粗提物中分离制备得到23-乙酰泽泻醇B 40.2 mg。结论建立的MPLC合p-HPLC法简便、快捷、高效地获得泽泻中23-乙酰泽泻醇B对照品。

Objective To establish a method for preparation of alisol B 23-acetate from rhizoma alismatis. Methods MPLC combined with p-HPLC were adopted. A MPLC was performed on silica gel column （3 cm × 13 cm, 40 g） with gradient elution of ligarine-acetic ether as mobile phase, and the flow rate was 50 mL.min-1. A p-HPLC was performed on Ultimate XB-C18 （21.2 mm×250 mm, 10 μm） with gradient elution of acetonitrile-water （65：35） as mobile phase, the flow rate was 15 mL.min-1, and the detective wavelength was 208 nm. Results 40.2 mg alisol B 23-acetate was separated and obtained once from 2 g ethyl acetate crude extract of rhizoma alismatis by MPLC combined with p-HPLC. Conclusion The method is simple, rapid and efficient, and can be applied to obtain alisol B 23-acetate from rhizoma alismatis.