高速逆流色谱分离纯化钩吻中钩吻素己和1-甲氧基钩吻碱  

Isolation and purification of gelsenicine and gelsevirine from Gelsemium elegans by high-speed counter-current chromatography

作　　者：沈洁[1] 苏燕评[1] 许盈[1] 刘浩[1] 刘铭[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

出　　处：《中草药》2009年第9期1392-1395,共4页Chinese Traditional and Herbal Drugs

基　　金：福建省科技计划重点项目(2007Y0018);福建医科大学教授学术发展基金资助项目(JS06027)

摘　　要：目的建立高速逆流色谱技术分离纯化钩吻素己和1-甲氧基钩吻碱的方法。方法采用高速逆流色谱分离技术分离纯化钩吻生物碱单体,以氯仿-甲醇-0.1mol/LHCl(4:4:2)为溶剂体系;高效液相色谱技术分析所提产物的质量分数;核磁共振谱、质谱分析确证单体的化学结构。结果从300mg钩吻总碱中经过一次高速逆流色谱技术分离纯化获得19.4mg钩吻素己和21.2mg1-甲氧基钩吻碱,质量分数分别为95.4%、98.6%;经过电喷雾质谱及核磁共振的结构鉴定分析,证实分离得到的两种生物碱分别是钩吻素己和1-甲氧基钩吻碱。结论高速逆流色谱技术可高效分离纯化钩吻素己和1-甲氧基钩吻碱,为钩吻生物碱的研发提供了制备技术。Objective To establish a new technique of high-speed counter-current chromatography （HSCCC） for isolation and purification of gelsenicine and gelsevirine. Methods The compounds were isolated and purified by HSCCC, using chloroform-methanol-0.1 mol/L hydrochloric acid （4 ： 4 ： 2） as the two-phase solvent system. The purity of the compounds was analyzed by HPLC. The structures of the compounds were confirmed by ESI-MS, ^1H-NMR, and ^13 C-NMR. Results Gelsenicine （19.4 mg） and gelsevirine （21.2 mg） were successfully obtained from crude extract （300 mg） of G. elegans in one-step separation, with purities of 95.4% and 98.6% by HPLC, respectively. The structures of gelsenicine and gelsevirine were identified by ESI-MS, ^1H-NMR, and ^13C NMR. Conclusion These results indicate that HSCCC is a very powerful technique for the isolation and purification of gelsenicine and gelsevirine.

关 键 词：钩吻 钩吻素己 1-甲氧基钩吻碱 高速逆流色谱 

分 类 号：R284.2[医药卫生—中药学] R286.02[医药卫生—中医学]