Separation and purification of four compounds from Desmodium styracifolium using off-line two-dimensional high-speed counter-current chromatography
Separation and purification of four compounds from Desmodium styracifolium using off-line two-dimensional high-speed counter-current chromatography
复制标题
离线二维高速逆流色谱法分离纯化广金钱草中四种化合物
DOI：
10.1002/jssc.201300653
复制
发表时间：
2013-10-01
影响因子：
3.1
通讯作者：
Chen, Xiaoqing
中科院分区：
文献类型：
--
作者：
Su, Wen;Liu, Qi;Chen, Xiaoqing
采用离线二维高速逆流色谱技术，成功分离纯化广金钱草乙酸乙酯提取物中的主要化合物。采用正己烷/乙酸乙酯/甲醇/水组成的两相溶剂体系，体积比为1：2：1：2（v/v/v/v）。以常规高速逆流色谱为第一维，溶剂体系的上相为固定相，采用头-尾洗脱模式，流速为2.0 mL/min，转速为900 rpm。再循环高速逆流色谱作为第二维，以分离第一维的不纯部分。共得到4个分离良好的物质，包括香草酸（1），-谷甾醇（2），芒柄花素（3），和芳香藤素（4），并通过HPLC-MS和H-1 NMR光谱鉴定其纯度和结构。结果表明，离线二维高速逆流色谱是分离复杂样品中化合物的有效方法。
An off-line 2D high-speed counter-current chromatography technique in preparative scale has been successfully applied to separate and purify the main compounds from the ethyl acetate extract of Desmodium styracifolium. A two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water at an optimized volume ratio of 1:2:1:2 v/v/v/v was used. Conventional high-speed counter-current chromatography was used as the first dimension, and the upper phase of the solvent system was used as the stationary phase in the head-to-tail elution mode at a flow rate of 2.0 mL/min and a rotation speed of 900 rpm. Recycling high-speed counter-current chromatography served as the second dimension to separate an impure fraction of the first dimension. A total of four well-separated substances including vanillic acid (1), -sitosterol (2), formononetin (3), and aromadendrin (4) were obtained, and their purities and structures were identified by HPLC-MS and H-1 NMR spectroscopy. The results illustrated that off-line 2D high-speed counter-current chromatography is an effective way to isolate compounds in complex samples.