HSCCC法结合制备型HPLC技术靶向制备分离与鉴定大血藤中的多酚类化合物

Preparative Isolation and Purification of Polyphenols from Daxueteng(Sargentodoxa Cuneata) by High Speed Counter-Current Chromatography Combined with Prep-HPLC

目的:建立大血藤中多种多酚类化合物高效稳定的制备分离方法。方法:以正己烷-乙酸乙酯-甲醇-水(3∶7∶4∶6,v/v)为溶剂体系,利用高速逆流色谱对大血藤正丁醇萃取物进行纯化,再结合制备型液相色谱获得各单体化合物,根据UV、MS、1H-NMR波谱信息确定化学结构。结果:从大血藤中分离鉴定了8个多酚类成分,分别为:(1)没食子酸;(2)原儿茶酸;(3)绿原酸;(4)咖啡酸;(5)香草酸;(6)阿魏酸;(7)异丹叶大黄素;(8)赤松素。化合物(7)(8)为首次从该属植物中分得。结论:高速逆流色谱和制备型液相色谱联用技术可高效制备分离大血藤中多种多酚类化合物,为大血藤的药理研究及质量控制奠定了基础。

Objective:To establish a new technique for isolation and purification of polyphenols from Daxueteng (Sargentodoxa Cuneata).Methods:In n-hexane:ethyl acetate:methanol:water (3:7:4:6)solvent system, polyphenols were isolated by high-speed counter current chromatography from n-butanol extract of Daxueteng (Sargentodoxa Cuneata),then the compounds of polyphenols purified by the prepared HPLC,and the structures were established on the basis of UV,MS and 1H-NMR.Results:A total of eight polyphenols were isolated and identified as gallic acid (1),protocatechuic acid (2),chlorogenic acid (3),caffeic acid (4),vanillic acid (5),ferulic acid (6),isorhapontigenin (7)and pinosylvin (8),respectively.Compounds (7)and (8)are isolated from the Daxueteng (Sargentodoxa Cuneata)for the first time.Conclusion:The results indicated that the proposed method could be widely applied for isolation of polyphenols from complex extracts.