高速逆流色谱法对当归中石油醚萃取部位化学成分的分离纯化  

Isolation and Purification of Four Active Components from Radix Angelicae sinensis by High-speed Counter-current Chromatography

作　　者：谢贵香[1] 王兵[1] 梁逸曾[1] 杨朝晖[1] 

机构地区：[1]中南大学化学化工学院中药现代化研究中心,湖南长沙410083

出　　处：《分析测试学报》2010年第10期1063-1067,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20875104);科技部国际合作项目(2007DFA40680)

摘　　要：采用高速逆流色谱法对当归石油醚萃取部位中4个主要化学成分进行分离纯化。选择Arizona溶剂体系作为高速逆流色谱分离的溶剂系统,经过实验条件优化,确定最佳溶剂为:正己烷-乙酸乙酯-甲醇-水(体积比6∶0.6∶3∶1)。高速逆流色谱分离时,采用有机相(上相)为固定相,水相(下相)为流动相,正相洗脱,流速为2mL/min,转速为900r/min,检测波长为254nm。当归石油醚萃取部位中的4种化学成分获得较好分离,经高效液相色谱检测,其纯度分别为78.5%、93.2%、98.9%、88.7%。通过1HNMR、IR和质谱分析,鉴别出其中1种化合物为藁本内酯。A high-speed counter-current chromatographic（HSCCC）method was applied in the systematic separation and purification of 4 main chemical components from the petroleum ether fraction of Radix Angelicae sinensis extracts.The separation of targeted compounds was performed by using the optimized solvent system consisting of n-hexane-ethyl acetate-methanol-water（6∶0.6∶3∶1,by volume）,and four fractions of high-speed counter-current chromatography were analyzed by high performance liquid chromatography.During the separation procedure,organic phase and water were used as stationary and mobile phase,respectively,with flow rate of 2 mL/min and 900 r/min rotation speed for HSCCC.The purities of the four compounds were 78.5%,93.2%,98.9%,88.7%,respectively,in which one was identified as ligustilide by 1H NMR,MS and IR spectra.

关 键 词：当归 高速逆流色谱 分离纯化 石油醚萃取 

分 类 号：O657.72[理学—分析化学] O652.6[理学—化学]