液相微萃取/后萃取技术在中药苯丙酸类化合物分析中的应用  

Application of Liquid Phase Microextraction with Back Extraction in the Analysis of Phenylpropionic Acids

作　　者：王晓园[1] 陈璇[1] 白小红[1] 

机构地区：[1]山西医科大学药学院,太原030001

出　　处：《分析化学》2009年第1期35-40,共6页Chinese Journal of Analytical Chemistry

基　　金：山西省自然科学基金(No.2007011086)资助项目

摘　　要：初步阐明了液相微萃取/后萃取(LPME/BE)在苯丙酸类化合物中的萃取机理;建立了浓缩倍数与模型化合物分配系数及理化参数之间的关系。利用自制的液相微萃取装置,优化了LPME/BE条件:以聚偏氟乙烯纤维(MOF503)为溶剂载体,正庚醇为萃取剂,pH3.0的HCl分析物水溶液为供相,pH11.7的NaOH为接受相,搅拌速度为1800r/min,萃取时间为60min。萃取完成后经HPLC分析。模型化合物浓缩倍数EF与其正庚醇/水表观油水分配系数logP有良好线性,R2=0.9653。测得该方法的RSD内<6.3%,RSD间<6.6%;检出限为咖啡酸0.025μg/L;阿魏酸0.250μg/L;对羟基桂皮酸0.004μg/L;对甲氧基桂皮酸0.100μg/L;桂皮酸0.050μg/L。双黄连口服液中咖啡酸平均回收率为100.3%;浓缩当归丸中阿魏酸平均回收率为99.2%;桂枝茯苓丸中桂皮酸平均回收率为99.4%。本法操作简便、快速、环境友好,能有效去除中药样品中复杂机体的干扰。Extraction mechanism of liquid phase microextraction with back extraction（LPME/BE） was elucidated initially. The relationships of concentration multiple and distribution coefficient and physico-chemical parameters were established. Analytes were extracted by a self-made LPME system and analyzed by HPLC. The optimal extraction conditions were as follows： polyvinylidene difluoride fibre as solvent carrier, n-enathol as organic solvent, HCl at pH 3.0 as donor phase and NaOH at pH 11.7 as acceptor phase, 1800 r/min of the stirring rate, and 60 min of the extraction time. The concentration multiple（EF） has good dependability with n-enanthol-water partition coefficient, R^2 =0. 9653. The intra-day precisions were lower than 6.3% and inter-day precisions were lower than 6.6%. The detection limit was 0. 025 g/L of caffeic acid, 0. 250 g/L for ferulic acid, 0. 004 g/L for P-hydroxycinnamic acid, 0. 100 g/L of methoxy cinnamic acid and 0. 050 g/L of cinnamic acid. The average recovery of caffeic acid in the Shuanghuanglian peroral liquid was 100.3%. The average recovery of ferulic acid in the Danggui concentrate pellet was 99.2% , and the average recovery of cinnamic acid in the Guizhifuling pellet was 99.4%. LPME/BE was applied to eliminate the interference of matrices, and to decrease the volume of use of organic solvent. The method shows the possibility for the deter- mination of bioactive compounds in traditional Chinese medicines. It is a quick and efficient pre-processing technique.

关 键 词：液相微萃取/后萃取 高效液相色谱 苯丙酸类化合物 萃取机理 分离优化模型 

分 类 号：R284.1[医药卫生—中药学]