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Simple analytical method for determination of pesticide residues in human serum by liquid chromatography tandem mass spectrometry

机译:液相色谱-串联质谱法测定人血清中农药残留的简单分析方法

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The aim of this study was to develop an analytical method for the determination of residues of organophosphorus and carba-mate pesticides which are widely used in Tunisia. This method involves a liquid-liquid extraction procedure followed by liquid chromatography tandem mass spectrometry (LC/MS/MS) for the identification and quantification of compounds. Ionization of molecules was performed by the electrospray mode. Multiple reactions monitoring (MRM) was the acquisition mode used for the monitoring of two MS/MS transitions for each compound. The average recoveries obtained, at three different fortification levels, ranged between 65% and 106% for most of the pesticides studied, except for methamidophos (lower than 25%).The linearity of the method was in the range of 5 to 50 μg/L with a correlation coefficient from 0.995 to 0.999, depending on the analyte. The estimated limit of detection and limit of quantification were 2 μg/L and 5 μg/L, respectively. The precision of the analytical procedure was satisfactory and the coefficients of variation, evaluated at three concentration levels were lower than 15% for most pesticides studied. The application of the method was investigated in a population of agricultural workers chronically exposed to various pesticides some of which, such as carbofuran, carbendazim, methomyl and pirimicarb, were detected in some serum samples.
机译:这项研究的目的是开发一种测定突尼斯广泛使用的有机磷和氨基甲酸酯类农药残留的分析方法。此方法涉及液-液萃取程序,然后进行液相色谱串联质谱分析(LC / MS / MS),以鉴定和定量化合物。分子的电离通过电喷雾模式进行。多反应监测(MRM)是用于监测每种化合物的两次MS / MS转换的采集模式。除甲胺磷(低于25%)外,大多数研究农药在三种不同的强化水平下获得的平均回收率在65%至106%之间。该方法的线性范围为5至50μg/ L的相关系数取决于分析物,其相关系数为0.995至0.999。估计的检出限和定量限分别为2μg/ L和5μg/ L。对于大多数研究的农药,在三个浓度水平下评估的分析程序的精度都令人满意,变异系数也低于15%。在长期暴露于各种农药的农业工人群体中研究了该方法的应用,其中一些血清样品中检出了某些农药,如呋喃丹,多菌灵,灭多威和吡虫威。

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