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建立一种改良的 QuEChERS 方法,结合 GC-MS 和 UPLC-MS/MS 用于人发中多类农药的分析。

Development of a modified QuEChERS method for multi-class pesticide analysis in human hair by GC-MS and UPLC-MS/MS.

机构信息

École Polytechnique Fédérale de Lausanne, Central Environmental Laboratory, Station 2, CH-1015 Lausanne, Switzerland.

出版信息

Anal Chim Acta. 2018 Jan 25;999:87-98. doi: 10.1016/j.aca.2017.11.009. Epub 2017 Nov 9.

Abstract

The present study assessed the suitability of using QuEChERS procedure for the simultaneous determination and quantification of 37 multi-class pesticides in human hair. Matrix co-eluted material had a large influence on instrumental response sensitivity. Purification was needed although dSPE cleanup sorbent selection critically influenced analyte recovery. Optimized protocol using Z-Sep+ sorbent successfully achieved recovery of 28 pesticides with high sensitivity, precision, and accuracy. Limits of detection ranged from 0.2 to 86.6 pg mg and from 0.5 to 6.3 pg mg for GC and UPLC amenable substances respectively. Pyrethroid pesticides were the most influenced by matrix effects which explained the higher limits of quantification retained for these substances. On the contrary, high sensitivity was achieved for UPLC amenable substances (LOD < 1 pg mg for atrazine, deisopropylatrazine, desethylatrazine, and imidacloprid). Suitability for monitoring pesticide exposure was assessed by application of the proposed protocol to samples collected on the field. Hairs of the volunteers were found positive to 8 pesticides with every sample containing at least one residue. Among these pesticides, only 3 were reported as used in local vegetable production, which suggested other sources of exposure. The developed method offers a sensitive, robust, and accessible tool for biomonitoring of human exposure.

摘要

本研究评估了 QuEChERS 程序用于同时测定和定量分析人发中 37 种多类农药的适用性。基质共洗脱物质对仪器响应灵敏度有很大影响。尽管 dSPE 净化吸附剂的选择对分析物回收率有很大影响,但仍需要进行净化。使用 Z-Sep+ 吸附剂优化的方案成功地实现了 28 种农药的高灵敏度、精密度和准确度回收。GC 和 UPLC 可分析物质的检测限分别为 0.2 至 86.6 pg mg 和 0.5 至 6.3 pg mg。拟除虫菊酯类农药受基质效应影响最大,这解释了这些物质保留的较高定量限。相反,UPLC 可分析物质的灵敏度很高(阿特拉津、去异丙基莠去津、去乙基莠去津和吡虫啉的检测限 < 1 pg mg)。通过将所提出的方案应用于现场采集的样品来评估监测农药暴露的适用性。志愿者的头发对 8 种农药呈阳性,每个样本至少含有一种残留。在这些农药中,只有 3 种被报道用于当地蔬菜生产,这表明存在其他来源的暴露。所开发的方法为人体暴露的生物监测提供了一种灵敏、稳健和易于使用的工具。

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