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使用低毒性溶剂的涡旋辅助液液微萃取结合高效液相色谱法测定水样中的五种有机磷农药

Vortex-assisted liquid-liquid microextraction using a low-toxicity solvent for the determination of five organophosphorus pesticides in water samples by high-performance liquid chromatography.

作者信息

Peng Guilong, He Qiang, Mmereki Daniel, Zhou Guangming, Pan Weiliang, Gu Li, Fan Leilei, Tang Xiaohui, Chen Junhua, Mao Yufeng

机构信息

Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, China.

National Centre for International Research of Low Carbon and Green Buildings, Chongqing University, Chongqing, China.

出版信息

J Sep Sci. 2015 Oct;38(20):3487-93. doi: 10.1002/jssc.201500547. Epub 2015 Sep 7.

Abstract

Vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with UV detection was applied to determine Isocarbophos, Parathion-methyl, Triazophos, Phoxim and Chlorpyrifos-methyl in water samples. 1-Bromobutane was used as the extraction solvent, which has a higher density than water and low toxicity. Centrifugation and disperser solvent were not required in this microextraction procedure. The optimum extraction conditions for 15 mL water sample were: pH of the sample solution, 5; volume of the extraction solvent, 80 μL; vortex time, 2 min; salt addition, 0.5 g. Under the optimum conditions, enrichment factors ranging from 196 to 237 and limits of detection below 0.38 μg/L were obtained for the determination of target pesticides in water. Good linearities (r > 0.9992) were obtained within the range of 1-500 μg/L for all the compounds. The relative standard deviations were in the range of 1.62-2.86% and the recoveries of spiked samples ranged from 89.80 to 104.20%. The whole proposed methodology is simple, rapid, sensitive and environmentally friendly for determining traces of organophosphorus pesticides in the water samples.

摘要

采用涡旋辅助液液微萃取结合高效液相色谱-紫外检测法测定水样中的水胺硫磷、甲基对硫磷、三唑磷、辛硫磷和甲基毒死蜱。以1-溴丁烷作为萃取溶剂,其密度高于水且毒性较低。该微萃取过程无需离心和分散剂。15 mL水样的最佳萃取条件为:样品溶液pH值为5;萃取溶剂体积为80 μL;涡旋时间为2 min;加盐量为0.5 g。在最佳条件下,测定水中目标农药时的富集因子在196至237之间,检测限低于0.38 μg/L。所有化合物在1-500 μg/L范围内均具有良好的线性关系(r>0.9992)。相对标准偏差在1.62-2.86%范围内,加标样品的回收率在89.80至104.20%之间。所提出的整个方法简单、快速、灵敏且对环境友好,适用于测定水样中的痕量有机磷农药。

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