Cao X, Tian Y, Zhang T Y, Ito Y
Beijing Institute for New Technology Application, China.
J Chromatogr A. 1998 Jul 17;813(2):397-401. doi: 10.1016/s0021-9673(98)00360-4.
High-speed counter-current chromatography (HSCCC) was used for the separation and purification of 10-deacetylbaccatin III from the needle extract of Chinese yew (Taxus chinensis). The crude needle extract (500 mg/5 ml) was first separated with a two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (2:5:2:5, v/v) and the partially purified fraction was again purified with a different solvent system composed of n-hexane-chloroform-methanol-water (5:25:34:20, v/v). HPLC analysis of the final fraction showed that the purity of 10-deacetylbaccatin (20 mg) was over 98%. The chemical structure was confirmed by fast atom bombardment MS and 1H NMR.
采用高速逆流色谱法(HSCCC)从中国红豆杉(Taxus chinensis)针叶提取物中分离纯化10-去乙酰巴卡亭III。首先将粗针叶提取物(500 mg/5 ml)用正己烷 - 乙酸乙酯 - 乙醇 - 水(2:5:2:5,v/v)组成的两相溶剂系统进行分离,然后将部分纯化的馏分再用由正己烷 - 氯仿 - 甲醇 - 水(5:25:34:20,v/v)组成的不同溶剂系统进行纯化。对最终馏分的HPLC分析表明,10-去乙酰巴卡亭(20 mg)的纯度超过98%。通过快原子轰击质谱和1H NMR对化学结构进行了确证。