State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Chaoyang District, Beijing, P. R. China.
J Sep Sci. 2011 Dec;34(23):3426-32. doi: 10.1002/jssc.201100547. Epub 2011 Nov 3.
Three active compounds, senkyunolide-I, senkyunolide-H and ferulic acid (FA), were successfully isolated and purified from the extracts of Rhizoma Chuanxiong by counter-current chromatography (CCC). Based on the principle of the partition coefficient values (k) for target compounds and the separation factor (α) between target compounds, the two-phase solvent system that contains n-hexane-ethyl acetate-methanol-water at an optimized volume ratio of 3:7:4:6 v/v was selected for the CCC separation, and the lower phase was employed as the mobile phase in the head-to-tail elution mode. In a single run, 400 mg of the crude extract yielded pure senkyunolide-I (6.4 mg), senkyunolide-H (1.7 mg) and FA (4.4 mg) with the purities of 98, 93 and 99%, respectively. The CCC fractions were analyzed by high-performance liquid chromatography, and the structures of the three active compounds were identified by MS and (1)H NMR.
三种活性化合物，即藁本内酯-I、藁本内酯-H 和阿魏酸（FA），已成功从川芎提取物中通过逆流色谱（CCC）分离和纯化。基于目标化合物的分配系数值（k）和目标化合物之间的分离因子（α）的原理，选择包含正己烷-乙酸乙酯-甲醇-水的两相溶剂系统，其优化的体积比为 3:7:4:6 v/v，用于 CCC 分离，并且下相在从头至尾洗脱模式下用作流动相。在单次运行中，从 400 毫克粗提取物中获得了纯度分别为 98%、93%和 99%的纯藁本内酯-I（6.4 毫克）、藁本内酯-H（1.7 毫克）和 FA（4.4 毫克）。通过高效液相色谱分析 CCC 馏分，并通过 MS 和（1）H NMR 鉴定三种活性化合物的结构。
