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涡旋辅助液-液微萃取结合气相色谱-质谱法测定环境水样和葡萄酒中的有机磷农药。

Vortex-assisted liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the determination of organophosphate pesticides in environmental water samples and wines.

机构信息

Research Laboratory for the Physical and Chemical Testing of Foods, Department of Food Technology, School of Food Technology and Nutrition, Alexander Technological Educational Institute (ATEI) of Thessaloniki, Thessaloniki, Greece.

出版信息

J Sep Sci. 2012 Sep;35(18):2422-9. doi: 10.1002/jssc.201200309. Epub 2012 Aug 15.

Abstract

A simple vortex-assisted liquid-liquid microextraction protocol followed by GC-MS is proposed for the determination of 12 organophosphate pesticides residues in environmental water samples and wines. The sample pretreatment employs the usage of low-density organic solvent. The parameters affecting the extraction efficiency (type and volume of organic extraction solvent, sample pH, ionic strength, extraction time, and centrifugation speed) were carefully examined. A mild emulsification process was involved by the addition of 40 μL toluene into 10 mL sample followed by sequential vortex-based agitation and manual shaking for 3 min. Following the extraction, the pesticide-rich organic solvent was recovered by centrifugation at 4000 rpm for 5 min. A fraction of the floated toluene was then collected and analyzed by GC-MS in SIM mode. Under the optimized conditions, the enrichment factor ranged between 65 and 389. Satisfactory linearity was observed for all pesticides tested with correlation coefficients higher than 0.9945 while the LODs were in the range of 2-11 ng L(-1) . The main advantages of the proposed method are the simplicity of operation, rapidity, low cost, and high sensitivity.

摘要

本文提出了一种简单的涡旋辅助液-液微萃取方案,结合 GC-MS 用于测定环境水样和葡萄酒中的 12 种有机磷农药残留。样品预处理采用低比重有机溶剂。仔细考察了影响萃取效率的参数(有机萃取溶剂的类型和体积、样品 pH 值、离子强度、萃取时间和离心速度)。通过向 10 mL 样品中加入 40 μL 甲苯,并进行连续涡旋搅拌和手动摇动 3 分钟,引入了温和的乳化过程。萃取后,将富含农药的有机溶剂在 4000 rpm 下离心 5 min 回收。然后取一部分浮在上面的甲苯,用 GC-MS 在 SIM 模式下进行分析。在优化条件下,所有测试农药的富集因子在 65 至 389 之间。所有农药的线性关系良好,相关系数均高于 0.9945,检出限范围为 2-11ng/L。该方法的主要优点是操作简单、快速、成本低、灵敏度高。

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