Liu Renmin, Li Aifeng, Sun Ailing
Department of Chemistry, College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng, Shandong, PR China.
J Chromatogr A. 2004 Oct 15;1052(1-2):223-7. doi: 10.1016/j.chroma.2004.08.127.
A preparative high-speed counter-current chromatography (HSCCC) method for isolation and purification of coumarins from Angelica dahurica (Fisch. ex Hoffin) Benth, et Hook. f(Baizhi in Chinese) was successfully established by using n-hexane-methanol-water as the two-phase solvent system in gradient elution mode. The upper phase of n-hexane-methanol-water (5:5:5, v/v) was used as the stationary phase of HSCCC. The mobile phase used in HSCCC was the lower phase of n-hexane-methanol-water (5:5:5, v/v) and n-hexane-methanol-water (5:7:3, v/v) that was changed in gradient. Three major components including imperatorin, isoimperatorin and oxypeucedanine were isolated, each at over 98% purity as determined by high-performance liquid chromatography (HPLC). The peak fractions of HSCCC were identified by 1H-NMR and 13C-NMR.
采用正己烷 - 甲醇 - 水作为两相溶剂体系，以梯度洗脱模式成功建立了一种从白芷（Angelica dahurica (Fisch. ex Hoffin) Benth, et Hook. f）中分离纯化香豆素的制备型高速逆流色谱（HSCCC）方法。正己烷 - 甲醇 - 水（5:5:5，v/v）的上相用作HSCCC的固定相。HSCCC中使用的流动相是正己烷 - 甲醇 - 水（5:5:5，v/v）和正己烷 - 甲醇 - 水（5:7:3，v/v）的下相，且呈梯度变化。分离得到了欧前胡素、异欧前胡素和氧化前胡素三种主要成分，通过高效液相色谱（HPLC）测定，每种成分的纯度均超过98%。HSCCC的峰馏分通过¹H-NMR和¹³C-NMR进行鉴定。
