Han Quan-Bin, Wong Lina, Yang Nian-Yun, Song Jing-Zheng, Qiao Chun-Feng, Yiu Hillary, Ito Yoichiro, Xu Hong-Xi
Chinese Medicine Laboratory, Hong Kong Jockey Club Institute of Chinese Medicine, Hong Kong, China.
J Sep Sci. 2008 Apr;31(6-7):1189-94. doi: 10.1002/jssc.200700582.
A simple method was developed to optimize the solvent ratio of the two-phase solvent system used in the high-speed counter-current chromatography (HSCCC) separation. Some mathematic equations, such as the exponential and the power equations, were established to describe the relationship between the solvent ratio and the partition coefficient. Using this new method, the two-phase solvent system was easily optimized to obtain a proper partition coefficient for the CCC separation of the target compound. Furthermore, this method was satisfactorily applied in determining the two-phase solvent system for the HSCCC preparation of pseudolaric acid B from the Chinese herb Pseudolarix kaempferi Gordon (Pinaceae). The two-phase solvent system of n-hexane/EtOAc/MeOH/H(2)O (5:5:5:5 by volume) was used with a good partition coefficient K = 1.08. As a result, 232.05 mg of pseudolaric acid B was yielded from 0.5 g of the crude extract with a purity of 97.26% by HPLC analysis.
开发了一种简单的方法来优化高速逆流色谱(HSCCC)分离中使用的两相溶剂系统的溶剂比。建立了一些数学方程,如指数方程和幂方程,以描述溶剂比与分配系数之间的关系。使用这种新方法,可以轻松优化两相溶剂系统,以获得用于目标化合物CCC分离的合适分配系数。此外,该方法成功应用于确定从中国草药金钱松(松科)中制备土槿皮酸B的HSCCC的两相溶剂系统。使用正己烷/乙酸乙酯/甲醇/水(体积比5:5:5:5)的两相溶剂系统,分配系数K = 1.08良好。结果,从0.5 g粗提取物中得到232.05 mg土槿皮酸B,通过HPLC分析纯度为97.26%。