薄层色谱-荧光法测定黄连生物碱分配系数  

Determination of Partition Coefficient of Alkaloids from Coptis Chinensis Franch by Thin Layer Chromatograph-Fluorometric Spectrophotometry

作　　者：贺凯[1] 李学刚[2] 陈红英[2] 叶小利[1] 邓亚飞[2] 陈新[2] 孙胜亮[1] 

机构地区：[1]西南大学生命科学学院,重庆400715 [2]西南大学药学院药用资源化学研究所,重庆400716

出　　处：《分析化学》2011年第4期572-575,共4页Chinese Journal of Analytical Chemistry

基　　金：国家科技部"重大新药创制"专项项目(No.2010ZX09401-306-3-10);重庆市十一五重大新药创制项目(No.2008AA5021);重庆科委攻关项目(No.CSTC2010AC5007);中央高校基本科研业务费专项(No.XDJK2009C095)资助

摘　　要：建立了薄层色谱和荧光分析法测定黄连生物碱在高速逆流色谱溶剂体系中分配系数的方法。样品在溶剂体系中分配平衡后,取等量的上下相,经点板、展开、刮板,提取后用荧光分光光度法检测样品的荧光值（激发波长365 nm,发射波长409 nm）,并计算样品在溶剂体系中的分配系数。在一定的浓度范围内,4种生物碱的含量与荧光强度呈良好的线性关系,加样回收率为94.7%~104.1%;相对标准偏差为1.9%~3.8%。本方法测定的分配系数与HPLC法无显著性差异。本方法准确度高,耗时少,应用范围广。A thin layer chromatograph（TLC） coupled with fluorometric spectrophotometric method has been established to determine the partition coefficient of alkaloids extracted from Coptis chinensis Franch in solvent systems of high speed counter-current chromatography（HSCCC）.After samples was equilibrated in solvent system,equal volume of upper and lower phase was spreaded with TLC method respectively and then extracted to measure the fluorescence intensity with fluorometric spectrophotometry（Lex 365 nm,Lem 409 nm） and to calculate the partition coefficient.A good linear relationship between fluorescence intensity and concentration of four kinds of alkaloid compounds in certain range was obtained.The average recoveries of epiberberine,coptisine,palmatine and berberine ranged from 94.7% to 104.1%.The range of relative standard deviations（RSD） in spiked samples was 1.9% to 3.8%.There was no significant difference in partition coefficient obtained with combined method,compared with HPLC.This method has high precision,broad applicability and consumes short time.

关 键 词：薄层色谱 荧光分析 高速逆流色谱 分配系数 溶剂体系 

分 类 号：R284.1[医药卫生—中药学]