酸水解结合高速逆流色谱分离制备高纯度牛蒡子苷元

Preparative Separation of High Purity Arctigenin from Arctii Fructus by Combining Acid Hydrolysis with HSCCC

建立酸水解结合高速逆流色谱法从牛蒡子中快速分离制备高纯度牛蒡子苷元的方法。采用醇提酸解法提取,再经氯仿萃取得牛蒡子粗提物;以石油醚-乙酸乙酯-甲醇-水(2∶5∶3∶4,v/v)作为两相溶剂系统,在流速10 m L/min、转速850 rpm、检测波长280 nm下实现对牛蒡子苷元的快速分离制备。80 min内从连续两次进样的1200 mg牛蒡子粗提物中分离得到牛蒡子苷元318 mg,其纯度达99.12%,得率达26.5%。该方法简便、快速、高效,可用于牛蒡子苷元的快速分离制备,为牛蒡子的开发利用提供了参考依据。

To establish a method for separating high purity arctigenin from Arctii Fructus by combining acid hydrolysis with high-speed counter-current chromatography （HSCCC）. The crude extract of Arctii Fructus was prepared by alcohol extraction and acid hydrolysis, followed by chloroform extraction. The separation conditions were as follows：the solvent system was petroleum ether-ethyl acetate-methyl-water （2： 5： 3： 4, v/v） where the upper phase was used as the stationa- ry phase and the lower phase as the mobile phase;the flow rate was 10.0 mL/min,the rotary speed was set at 850 rpm and the detection wavelength was 280 nm. As a result,318 mg of arctigenin with the purity of 99.12 % was separated from 1200 mg of crude sample within 80 minutes and the productive rate reached to 26.5%. The developed method was simple ,rapid and efficient. It was suitable for the preparative separation of arctigenin and provided a reference for the de- velopment and utilization of Arctii Fructus.