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离子液体-DLLME-HPLC测定小麦中有机氯农药
Determination of Three Organochlorine Pesticides by Ionic Liquid Based Dispersive Liquid-Liquid Microextraction Coupled with HPLC
【Author】 LIU Wei,HE Lijun~* (School of Chemistry and Chemical Engineering,Henan University of Technology,Zhengzhou 450001)
【机构】 河南工业大学化学化工学院;
【摘要】 离子液体-分散液液微萃取(ionicliquid-dispersive liquid liquid microextraction,IL-DLLME)结合了DLLME的简单快速及IL的稳定、萃取效果高的优点,已被成功用于各种有机或无机物质的分离富集。本文用含有1-苄基-3-甲基咪唑双三氟甲基磺酰亚胺离子液体的乙腈溶液,在磁力搅拌下,萃取小麦粉中的3种有机氯(2,4-DDE、2,4-DDT和4,4-DDE)。然后将一部分所得提取液加入5 mL二次蒸馏水中进行DLLME,离心后取底部沉积相进行HPLC分析。考察了影响萃取过程的各种因素,在优化条件下,对方法进行了评价。3种有机氯的富集倍数和萃取回收率范围分别是178~188及59.3%~63.5%,线性范围为0.1~100μg/g,RSD(n=5)为1.9%~7.4%,最小检测限(S/N=3)为1 ng/g。将此方法应用于3种不同年份收割的实际小麦样品,3种有机氯的RSD(n=3)和加标回收率范围分别为0.2%~6.5%和95.8%~126.4%。与其它传统萃取方法相比,本方法具有快速,使用溶剂剂量少,操作简便。
【Abstract】 In this work,three organochlorine pesticides(2,4-DDE,2,4-DDT and 4,4-DDE) in wheat power were analyzed using 1-benzyl-3-methylimidazolium bis[(trifluoromethyl) sulfonyl]imide ionic liquid-dispersive liquid-liquid extraction(IL-DLLME) coupled with HPLC.Experimental conditions affecting DLLME procedure were optimized.Under the optimized conditions,the enrichment factor and extraction recovery were in the range of 178~188 and 59.3%~63.5%,respectively.The linearity range of this method was 0.1~100μg/g with the RSD(n=5) of 1.9%~7.4%,and the detection limit was 1 ng/g.This method was applied to detect three real wheat samples which were harvested in different years,RSD(n=3) and relative recovery were in the range of 0.2%~6.5%and 95.8%~126.4%,respectively.The proposed method is quick,easy to operate and reduce the consumption of organic solvent compared with the conventional sample preparation method.
【Key words】 ionic liquid; dispersive liquid-liquid microextraction; organochlorine pesticide; wheat; HPLC;
- 【会议录名称】 中国化学会第十二届全国应用化学年会论文集
- 【会议名称】中国化学会第十二届全国应用化学年会
- 【会议时间】2011-10-17
- 【会议地点】中国河南郑州
- 【分类号】TS211.7;O657.72
- 【主办单位】中国化学会(The Chinese Chemical Society)、中国科学院长春应用化学研究所(The Changchun Institute of Applied Chemistry,CAS)