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Development and validation of a SPE-GC-MS method for the determination of pesticides in surface water

机译:SPE-GC-MS测定地表水中农药的方法的开发和验证

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摘要

A method for analysis of 20 commonly used pesticides in surface water based on solid-phase extraction and gas chromatography-mass spectrometry was proposed. During method development the key parameters that can affect SPE extraction and determination such as selection of efficient SPE sorbent, pH of water sample, type and volume of elution solvent, breakthrough volume and matrix effects were investigated. The method was validated using spring water spiked with appropriate concentration of pesticides. The obtained correlation coefficients were in range 0.9972-1.000, limits of detection (LOD) were 0.001-0.5 μg L~(-1) and the limits of quantification (LOQ) were 0.005-1 μg L~(-1) depending on a pesticide. Much higher LOD (20μg L~(-1)) and LOQ (50 μg L~(-1)) values were obtained for bentazone. The influence of matrix was assessed using real water samples spiked with appropriate concentration of pesticide standards solution. Both signal enhancement and suppression were observed, depending on a pesticide, therefore standard addition method was used for pesticides determination. The developed method was applied on real water samples taken in close vicinity of agricultural fields. Many of the targeted pesticides were found in the samples and the results are presented in this article.
机译:提出了一种基于固相萃取和气相色谱-质谱法分析地表水中20种常用农药的方法。在方法开发过程中,研究了可能影响SPE萃取和测定的关键参数,例如有效SPE吸附剂的选择,水样品的pH,洗脱溶剂的类型和体积,突破体积和基质效应。使用加有适当浓度农药的泉水对该方法进行了验证。所获得的相关系数在0.9972-1.000的范围内,检测限(LOD)为0.001-0.5μgL〜(-1),定量限(LOQ)为0.005-1μgL〜(-1),具体取决于农药。苯达松的LOD(20μgL〜(-1))和LOQ(50μgL〜(-1))值更高。使用掺有适当浓度农药标准溶液的真实水样评估基质的影响。观察到信号增强和抑制,这取决于农药,因此使用标准添加方法确定农药。所开发的方法应用于在农田附近采集的真实水样。在样品中发现了许多目标农药,结果在本文中介绍。

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