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基于涡旋辅助的低密度溶剂破乳分散液液微萃取和高效液相色谱法测定水样中的有机磷农药。

Vortex-assisted low density solvent based demulsified dispersive liquid-liquid microextraction and high-performance liquid chromatography for the determination of organophosphorus pesticides in water samples.

机构信息

Materials Chemistry Research Unit, Department of Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand.

Department of Chemistry, Faculty of Engineering, Rajamangala University of Technology Isan, Khon Kaen Campus, Khon Kaen 40000, Thailand.

出版信息

Chemosphere. 2014 May;103:51-8. doi: 10.1016/j.chemosphere.2013.11.024. Epub 2013 Dec 13.

Abstract

A simple, rapid, effective and eco-friendly preconcentration method, vortex-assisted low density solvent based solvent demulsified dispersive liquid-liquid microextraction (VLDS-SD-DLLME), followed by high performance liquid chromatography-diode array detector (HPLC-DAD) analysis, has been developed for the first time for the determination of four organophosphorus pesticides (OPPs) (e.g., azinphos-methyl, parathion-methyl, fenitrothion and diazinon) in environmental water samples. In this preconcentration procedure, an emulsion was obtained after the mixture of extraction solvent (1-dodecanol) and dispersive solvent (acetonitrile, ACN) was injected rapidly into 10 mL of the sample solution. The vortex agitator aided the dispersion of the extraction solvent into the sample solution. After the formation of an emulsion, the demulsifier (ACN) was added, resulting in the rapid separation of the mixture into two phases without centrifugation. Under optimal conditions, the proposed method provided high extraction efficiency (90-99%), good linearity range (0.5-500 ng mL(-1)), low limits of detection (0.25-1 ng mL(-1)) and good repeatability and recoveries were obtained.

摘要

一种简单、快速、有效且环保的预浓缩方法,涡旋辅助低密度溶剂基溶剂分散液液微萃取(VLDS-SD-DLLME),随后进行高效液相色谱-二极管阵列检测器(HPLC-DAD)分析,首次用于测定环境水样中的四种有机磷农药(OPPs)(如马拉硫磷、甲基对硫磷、杀螟硫磷和二嗪农)。在该预浓缩过程中,将萃取溶剂(1-十二醇)和分散溶剂(乙腈,ACN)的混合物快速注入 10 mL 样品溶液后,会得到乳液。涡旋搅拌器辅助萃取溶剂分散到样品溶液中。形成乳液后,加入破乳剂(ACN),无需离心即可快速将混合物分成两相。在最佳条件下,所提出的方法提供了高萃取效率(90-99%)、良好的线性范围(0.5-500ngmL(-1)))、低检测限(0.25-1ngmL(-1)))和良好的重现性和回收率。

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