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 13C-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

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)