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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of several pesticides in water by solid-phase extraction, liquid chromatography and electrospray tandem mass spectrometry
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Determination of several pesticides in water by solid-phase extraction, liquid chromatography and electrospray tandem mass spectrometry

机译:固相萃取,液相色谱和电喷雾串联质谱法测定水中的几种农药

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The analysis of pesticides in water samples is a problem of primary concern for quality control laboratories due to the toxicity level of these compounds and their public health risk. In order to evaluate the impact of pesticides in the Lisbon drinking water supply system, following the requirements of the European Union Directive 98/83/EC, we developed and validated an analytical method based on the combination of solid-phase extraction with liquid chromatography and tandem mass spectrometry. In this work, several pesticides were studied: imidacloprid, dimethoate, cymoxanil, carbendazime, phosmet, carbofuran, isoproturon, diuron, methidathion, linuron, pyrimethanil, methiocarbe, tebuconazole and chlorpyrifos. Several parameters of the electrospray source were optimized in order to get the best formation conditions of the precursor ion for each pesticide, namely capillary and extractor voltage, cone voltage, cone gas flow rate and desolvation gas flow rate. After optimization of the collision cell energy of the triple quadrupole, two different precursor ion - product ion transitions were selected for each pesticide, one for quantification and one for qualification, and these ions were monitored under time-scheduled multiple reaction monitoring (MRM) conditions. The selection of specific fragment ions for each pesticide guarantees a high degree of selectivity as well as additional sensitivity to quantify trace levels of these pesticides in water samples. This method showed excellent linearity ranges for all pesticides, with correlation coefficients greater than 0.9989. Determination limits (between 0.0041 and 0.0480 mu g/L), precision (RSD <9.18%), accuracy and recovery studies in several water samples using solid-phase extraction were also performed. (C) 2006 Elsevier B.V. All rights reserved.
机译:水样中农药的分析是质量控制实验室最关心的问题,因为这些化合物的毒性水平及其公共健康风险。为了评估农药对里斯本饮用水供应系统的影响,我们遵循欧盟指令98/83 / EC的要求,开发并验证了固相萃取与液相色谱结合的分析方法。串联质谱在这项工作中,对几种农药进行了研究:吡虫啉,乐果,灭草胺,多菌灵,磷酸二甲酯,呋喃丹,异丙隆,敌草隆,甲硫磷,利尿隆,嘧啶酮,甲硫威,戊唑醇和毒死rif。优化了电喷雾源的几个参数,以便获得每种农药的最佳前体离子形成条件,即毛细管和萃取器电压,锥孔电压,锥孔气体流速和去溶剂化气体流速。优化了三重四极杆的碰撞池能量后,为每种农药选择了两种不同的前体离子-产物离子跃迁,一种用于定量,一种用于鉴定,并且在定时多反应监测(MRM)条件下对这些离子进行了监测。为每种农药选择特定的碎片离子可确保高度的选择性以及定量水样品中这些农药的痕量水平的额外灵敏度。该方法对所有农药显示出极好的线性范围,相关系数大于0.9989。还进行了使用固相萃取的几种水样的测定限(0.0041至0.0480μg / L),精密度(RSD <9.18%),准确度和回收率研究。 (C)2006 Elsevier B.V.保留所有权利。

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