目的 建立应用高速逆流色谱技术分离纯化中国钩吻中钩吻素子的方法。方法 从中国钩吻中提取得到的钩吻总碱以氯仿-甲醇-0.1 mol/L HCl(4 ∶ 4 ∶ 2 ，V/V/V)为溶剂体系，通过高速逆流色谱进行分离，得到的目标单体采用高效液相色谱分析纯度，核磁共振谱氢谱、质谱分析确证化学结构。结果 进样300 mg钩吻总碱，分离得到生物碱单体为75 mg，经结构鉴定确证为钩吻素子，高效液相色谱分析得到质量分数为99.2 %。结论 高速逆流色谱技术可高效分离纯化钩吻素子。

Objective To develop a new method of high-speed counter-current chromatography(HSCCC) for separation and purification of koumine from Gelsemium elegans. Methods The crude extract of Gelsemium elegans was separated by HSCCC with the two-phase solvent system consisting of chloroform-methanol-0.1 mol/L hydrochloric acid(4∶4∶2 in volume ratio). The purity of the compound was analyzed by high performance liquid chromatography(HPLC).The chemical structure of the compound was confirmed by electrospray ionization-mass spectroscopy(ESI-MS)1H- nuclear magnetic resonance(NMR). Results Seventy-five mg of koumine was successfully obtained from 300 mg of the crude extract，and the structure was identified as koumine by ESI-MS and 1H-NMR. Its purity was 99.2 % showed by HPLC. Conclusion The HSCCC can be applied to separate and purify koumine powerfully.

R284.1

福建医科大学重大科研项目(ZD009)；福建省发展和改革委员会产业技术开发项目(闽发改投资[2009]958号)。