离子液体顶空单滴微萃取分析中药中的高沸点挥发性成分  

Ionic Liquid-Based Headspace Single Drop Microextraction for Analysis of Volatile Components with High Boiling Point in Traditional Chinese Medicines

作　　者：何小稳[1] 蒋晔[1] 刘彦[1] 

机构地区：[1]河北医科大学药学院,石家庄050017

出　　处：《分析化学》2010年第5期727-730,共4页Chinese Journal of Analytical Chemistry

基　　金：河北省自然科学基金(No.C2009001069)资助项目

摘　　要：建立了分析中药中高沸点挥发性成分的离子液体顶空单滴微萃取-液相色谱法,并用于复方鲜竹沥液中愈创木酚的含量的测定。采用改进的悬滴装置,增大了液滴与微量进样器针尖处塑料套管的接触面积,使离子液体的液滴达12μL,提高了液滴的稳定性及方法的灵敏度。考察并优化了影响萃取的因素,确定了萃取条件:以12μL1-丁基-3-甲基咪唑基六氟磷酸盐([BMIM][PF6])为悬滴,在5mL含36%(w/V)NaCl的样品溶液中,萃取温度80℃、搅拌速度1000r/min的条件下,顶空萃取30min,萃取后直接将液滴吸回微量进样器,进行HPLC检测。愈创木酚在0.05～1.6mg/L范围内线性关系良好(r=0.9997);检出限为0.39μg/L,愈创木酚的加样回收率为97.6%,RSD为2.5%。本方法操作简单、定量准确,样品前处理简单,成本低,无污染。An improved headspace single drop microextraction procedure using ionic liquid has been developed for the pretreatment of volatile components with high boiling point in traditional Chinese medicines. The procedure combined with high performance liquid chromatography was applied to the determination of guaiacol in compound succus bambusae oral solution. The volume of ionic liquid microdrop was increased to 12 μL by modifying the device of suspended drop to increase the contact area of the microdrop and the bottom of plastic tube to the tip of microsyringe needle. The stability of microdrop and the sensitivity of the method were improved. The variables affecting the extraction efficiency were optimized and the final extraction procedure was as follows： a 12-μL ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphat （[BMIM][PF6]） microdrop was exposed on the headspace above a 5-mL sample solution containing 36%（w/V） sodium chloride with a stirring rate of 1000 r/min at 80 ℃ for 30 min. After extraction, the microdrop was directly injected into HPLC for analysis. Under the optimum experimental conditions, a good linear relation was obtained in the range of 0.05-1.6 mg/L for guaiacol（r=0.9997）. The limit of detection was 0.39 μg/L and the average recovery was 97.6% with the relative standard deviations of 2.5%. The proposed method is simple, fast, accurate and inexpensive without complicated sample pretreatment and contamination.

关 键 词：离子液体 顶空单滴微萃取 高沸点挥发性成分 复方鲜竹沥液 愈创木酚 

分 类 号：TQ460.1[化学工程—制药化工]