Determination of 27 pesticides in wine by dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry
Determination of 27 pesticides in wine by dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry
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分散液液微萃取气相色谱-质谱法测定葡萄酒中27种农药
DOI：
10.1016/j.microc.2015.11.003
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发表时间：
2016-05-01
影响因子：
4.8
通讯作者：
Ouyang, Gangfeng
中科院分区：
文献类型：
--
作者：
Chen, Bo;Wu, Feng-qi;Ouyang, Gangfeng
建立了一种低溶剂消耗方法，采用分散液液微萃取 (DLLME) 测定葡萄酒中 27 种不同类别的农药（包括有机氯农药、有机磷农药、拟除虫菊酯农药、杀菌剂、除草剂和杀螨剂）。对提取溶剂的类型和体积、分散剂的类型和体积、盐度、pH、离心时间、涡流提取时间和酒体积等提取参数进行了优化。将60μL氯仿（提取溶剂）和940μL乙腈（分散溶剂）的混合物注入5mL酒稀释液中。振荡、离心后，将沉淀相转移至200μL玻璃插管中，采用气相色谱-质谱法（GC-MS）测定。结果表明，所有农药的回收率在三个不同水平上的峰值范围为 66.7% 至 126.1%。日内重复性 (RSD) 范围为 2.0% 至 27.2%。检测限为0.025～0.88μg/L，定量限为0.082～2.94μg/L。该方法成本低、快速、方便，可作为葡萄酒中多种农药监测的有效方法。 (C) 2015 Elsevier B.V. 保留所有权利。
A low solvent consumption method was developed to determine 27 different classes of pesticides (including organochlorine pesticide, organophosphorus pesticide, pyrethroid pesticide, fungicide, herbicide and acaricide) in wine using dispersive liquid-liquid microextraction (DLLME). Extraction parameters including type and volume of extraction solvent, type and volume of disperser solvent, salinity, pH, centrifugation time, vortex extraction time and wine volumes were optimized. A mixture of 60 mu L chloroform (extraction solvent) and 940 mu L acetonitrile (disperser solvent) was injected into 5 mL wine diluent. After shaking and centrifugation, the sedimented phase was transferred into a 200 mu L glass insert and determined by gas chromatography-mass spectrometry method (GC-MS). The results demonstrated that the recoveries for all the pesticides spiked at three different levels ranged from 66.7 to 126.1%. The intra-day repeatabilities (RSDs) ranged from 2.0 to 27.2%. The limits of detection ranged from 0.025 to 0.88 mu g/L, and the limits of quantification ranged from 0.082 to 2.94 mu g/L. The proposed method is very low cost, rapid and convenient, and could be an effective method for monitoring of multi-pesticide in wine. (C) 2015 Elsevier B.V. All rights reserved.