高速逆流色谱分离制备钩吻素子  

Separation and Purification of Koumine from Gelsemium elegans by High-speed Counter-current Chromatography

作　　者：刘浩[1,2] 沈洁[1] 刘铭[1] 许盈[1] 俞昌喜[1] 

机构地区：[1]福建医科大学药学院药理学系,福建福州350004 [2]武警福建总队医院药剂科,福建福州350003

出　　处：《中药新药与临床药理》2013年第2期197-200,共4页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：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)

摘　　要：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 HC(l4∶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 separa- tion and purification of koumine from Gelsemium elegans. Methods The crude extract of Gelsemium elegans was sep-arated 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 （ES- I-MS）IH- 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.

关 键 词：钩吻 钩吻素子 高速逆流色谱 分离纯化 

分 类 号：R284.1[医药卫生—中药学]