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离子液体介导的分子印迹固相萃取结合气相色谱-电子捕获检测器快速筛选蔬菜中的三氯杀螨醇。

Ionic liquid-mediated molecularly imprinted solid-phase extraction coupled with gas chromatography-electron capture detector for rapid screening of dicofol in vegetables.

机构信息

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China.

出版信息

J Chromatogr A. 2013 Sep 13;1307:21-6. doi: 10.1016/j.chroma.2013.07.054. Epub 2013 Jul 19.

Abstract

New ionic liquid-mediated molecularly imprinted polymers (IL-MIPs) were prepared by precipitation polymerization using 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM(+)PF6(-)) as the auxiliary solvent, α-chloro-DDT as the dummy template, and they were successfully applied as the sorbents of solid-phase extraction (SPE) for rapid screening of dicofol from cabbage, tomato, and carrot samples. The IL-MIPs were characterized by FTIR, FE-SEM, static adsorption and chromatographic evaluation, and the results revealed that the IL-MIPs had higher adsorption capacity and selectivity to dicofol in aqueous solution than that of ionic liquid-mediated non-imprinted polymers (IL-NIPs) and non-imprinted polymers (NIPs). Under the optimized conditions, the IL-MIPs-SPE-GC method offered good linearity (0.4-40.0ngg(-1), r(2)=0.9995) and the average recoveries of dicofol at three spiked levels were in a range of 84.6-104.1% (n=3) with RSD≤7.6%. The proposed method obviously improved the selectivity and purification effect, and eliminated the effect of template leakage on dicofol quantitative analysis.

摘要

新型离子液体介导的分子印迹聚合物(IL-MIPs)通过沉淀聚合制备,以 1-丁基-3-甲基咪唑六氟磷酸盐(BMIM(+)PF6(-))作为辅助溶剂,以α-氯-DDT 作为虚拟模板,并成功用作固相萃取(SPE)的吸附剂,用于从甘蓝、番茄和胡萝卜样品中快速筛选三氯杀螨醇。通过傅里叶变换红外光谱(FTIR)、场发射扫描电子显微镜(FE-SEM)、静态吸附和色谱评价对 IL-MIPs 进行了表征,结果表明,IL-MIPs 对水溶液中的三氯杀螨醇具有比离子液体介导的非印迹聚合物(IL-NIPs)和非印迹聚合物(NIPs)更高的吸附容量和选择性。在优化条件下,IL-MIPs-SPE-GC 方法具有良好的线性(0.4-40.0ngg(-1),r(2)=0.9995),三水平加标回收率在 84.6-104.1%(n=3)范围内,相对标准偏差(RSD)≤7.6%。该方法明显提高了选择性和净化效果,消除了模板泄漏对三氯杀螨醇定量分析的影响。

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