高速逆流色谱分离与鉴定牡荆化学成分  

Separation of Chemical Compounds in Vitex negundo L.by Preparative High-speed Counter-current Chromatography

作　　者：罗娅君[1] 边清泉[1] 张琦[2,3] 刘志荣[1] 张新申[3] 

机构地区：[1]绵阳师范学院化学与化学工程学院,四川绵阳621000 [2]西南民族大学生命科学与技术学院,四川成都610041 [3]四川大学轻纺与食品学院,四川成都610065

出　　处：《分析测试学报》2011年第9期1044-1049,共6页Journal of Instrumental Analysis

基　　金：国家"十一五"科技支撑计划资助项目(2006BAI06A18-15);四川省教育厅重点项目(092A180);绵阳师范学院科研资助项目(MA2009017)

摘　　要：采用制备型高速逆流色谱与高效液相色谱联用的方法分离纯化牡荆中的活性化学成分。通过对溶剂系统和参数条件的优化,获得较好的分离条件。溶剂体系:氯仿-甲醇-水(体积比4∶3∶2),上相(水相)为固定相,下相(有机相)为流动相,正相洗脱;进样质量浓度20 g.L-1;流速2.0 mL.min-1;转速850 r.min-1。进一步分离获得5个高纯度的化合物,经鉴定为牡荆素(Ⅰ)、紫花牡荆素(Ⅱ)、异绿原酸(Ⅵ)、木犀草素(Ⅶ)、木犀草素-7-O-β-D-葡萄糖苷(Ⅷ),其纯度分别为98.0%、92.3%、96.8%、97.4%、90.3%。Preparative high-speed counter-current chromatography（HSCCC） and high performance liquid chromatography（HPLC） were employed firstly to separate chemical compounds in Vitex negundo L..The procedure was performed in a two-phase solvent system of chloroform-methanol-water（4 ∶ 3 ∶ 2,by volume） at a flow rate of 2.0 mL·min^-1 by normal phase elution,in which the upper phase was the stationary phase and the lower phase was the mobile phase.The sample concentration was 20 g·L-1,while the rotation speed was 850 r·min^-1 and the eluate was detected at 254 nm.Five compounds were obtained from the crude extract of the plant in a simultaneous process,which,according to their physical and chemical properties,were identified as：vitexin（Ⅰ）,casticin（Ⅱ）,3,5-di-O-caffeylquinic acid（Ⅵ）,luteolin（Ⅶ）,luteolin-7-O-β-D-glucoside（Ⅷ）.The purities of the five compounds were 98.0%,92.3%,96.8%,97.4%and 90.3%,respectively.

关 键 词：高速逆流色谱 牡荆 高效液相色谱 化学成分 分离 

分 类 号：O657.72[理学—分析化学] J522.3[理学—化学]