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首页> 外文期刊>Journal of separation science. >Vortex-assisted liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the determination of organophosphate pesticides in environmental water samples and wines
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Vortex-assisted liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the determination of organophosphate pesticides in environmental water samples and wines

机译:涡流辅助液-液微萃取-气相色谱-质谱法测定环境水样和葡萄酒中的有机磷酸酯农药

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摘要

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.
机译:提出了一种简单的涡流辅助液-液微萃取方案,然后采用GC-MS测定环境水样品和葡萄酒中的12种有机磷酸酯农药残留。样品预处理采用了低密度有机溶剂。仔细检查了影响萃取效率的参数(有机萃取溶剂的类型和体积,样品的pH,离子强度,萃取时间和离心速度)。通过向10 mL样品中添加40μL甲苯,然后依次进行基于涡旋的搅拌和手动摇动3分钟,来进行温和的乳化过程。萃取后,通过以4000 rpm离心5分钟来回收富含农药的有机溶剂。然后收集一部分浮动的甲苯,并通过SIM模式的GC-MS分析。在优化的条件下,富集系数在65到389之间。所有被测农药的线性均令人满意,相关系数高于0.9945,而LODs在2-11 ng L〜(-1)范围内。所提出的方法的主要优点是操作简单,快速,低成本和高灵敏度。

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