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采用 QuEChERS 法结合电子捕获检测技术建立气相色谱法测定黄瓜中农药多残留的方法

Development and validation of gas chromatography with electron capture detection method using QuEChERS for pesticide residue determination in cucumber.

机构信息

Research Centre for Residue and Quality Analysis, Faculty of Horticulture, Sher-e-Kashmir University of Agricultural Sciences and Technology (SKUAST-K), Shalimar Campus, Srinagar, India.

Directorate of Research, Sher-e-Kashmir University of Agricultural Sciences and Technology (SKUAST-K), Shalimar Campus, Srinagar, India.

出版信息

Biomed Chromatogr. 2023 Aug;37(8):e5647. doi: 10.1002/bmc.5647. Epub 2023 Apr 25.

Abstract

A modified quick, easy, cheap, efficient, rugged, and safe (QuEChERS) method coupled to gas chromatography with electron capture detection was developed for the simultaneous determination of selected electronegative pesticides, namely, chlorpyrifos-methyl (1), chlorpyrifos (2), quinolphos (3), profenofos (4), myclobutanil (5), ethion (6), fenpropathrin (7), and cypermethrin (8), in vegetables with high water content. The selected compounds and some of their metabolites have even been found in human body fluids. In addition, some of them are known or suspected carcinogens according to the World Health Organization. Extraction and cleanup parameters were optimized; thus, the original QuEChERS method was modified to minimize solvent usage by making the study eco-friendly. The developed method was validated for selectivity, specificity, linearity, precision, and accuracy using SANTE guidelines. Calibration curves showed good linearity (r > 0.99) within the test range. Precision was evaluated by intra- and inter-day experiments with an acceptable range of less than 20.0% of relative standard deviation. Recovery was evaluated at limit of quantification and was found to be in the range of 70-120%, with relative standard deviations lower than 4.21%. The proposed method is applicable for detection and monitoring of selected pesticides in one run not only in fruits and vegetables with high water content but also in samples containing large quantities of pigments/dyes.

摘要

建立了一种改良的快速、简便、价廉、有效、耐用、安全(QuEChERS)方法,并将其与带有电子捕获检测的气相色谱法相结合,用于同时测定选定的电负性农药,即甲基毒死蜱(1)、毒死蜱(2)、喹硫磷(3)、丙溴磷(4)、咪鲜胺(5)、乙硫磷(6)、甲氰菊酯(7)和氯氰菊酯(8)在含水量高的蔬菜中的含量。已在人体体液中发现所选化合物及其一些代谢物。此外,根据世界卫生组织的规定,其中一些是已知的或可疑的致癌物。优化了提取和净化参数;因此,通过使研究更环保,对原始的 QuEChERS 方法进行了修改,以最小化溶剂的使用。根据 SANTE 指南,对所开发的方法进行了选择性、特异性、线性、精密度和准确度的验证。校准曲线在测试范围内表现出良好的线性(r>0.99)。通过日内和日间实验评估精密度,相对标准偏差在可接受范围内小于 20.0%。回收率在定量限进行评估,发现回收率在 70-120%之间,相对标准偏差低于 4.21%。该方法适用于在一次运行中检测和监测高含水量水果和蔬菜以及含有大量颜料/染料的样品中的选定农药。

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