高速逆流色谱结合粉末直接进样分离槐花中芦丁方法的建立

Preparative separation of rutin from Flos Sophorae by high-speed counter-current chromatography with injection of crude drugs' powder

[目的]建立以生药粉末为进样方式从槐花中直接分离制备芦丁的高速逆流色谱法。[方法]生药粉末直接进行高速逆流色谱(high-speed counter-current chromatography,HSCCC)分离纯化,以乙酸乙酯-正丁醇-水(2∶1∶3)为溶剂系统,下相为流动相,流速1.5 mL.min-1,检测波长254 nm,分离温度30℃,所得产物经高效液相色谱、紫外光谱与质谱分析检测,并与标准品对照。[结果]在此条件下,经一步分离从300 mg生药粉末中得到53mg纯度为95.4%的芦丁。[结论]该法简便、快速、所得产物纯度高,可用于芦丁快速制备。

[ Objective ] To develop a protocol of application high - speed counter - current chromatography （ HSCCC ） for the preparative separation of rutin from Flos Sophorae. [ Method] A two - phase solvent system composed of ethyl acetate： n - butanol： water （2： 1： 3 ） （V/V/V） was used, and the lower phase was used as the mobile phase at a flow rate of 1.5 mL · min ^-1. The apparatus and eluate were monitored at 830 r · min ^-1 and 254 nm, [ Result] Fifty - three mg rutin with purity of 95.4% determined by HPLC was obtained from 300 mg powder of crude drugs only in one - step separation. [ Conclusion] The established protocol is simple, high efficiency and suitable for the separation of rutin.