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建立并验证超高效液相色谱-串联质谱法同时检测死后检材中多种农药的方法。

Development and validation of a multi-substance method for routine analysis of pesticides in post-mortem samples by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry.

机构信息

Instituto Nacional de Medicina Legal e Ciências Forenses, I.P., Delegação do Sul, Portugal; Faculdade de Ciências e Tecnologia, Universidade de Coimbra, Portugal.

Instituto Nacional de Medicina Legal e Ciências Forenses, I.P., Delegação do Centro, Portugal.

出版信息

J Pharm Biomed Anal. 2024 Aug 1;245:116176. doi: 10.1016/j.jpba.2024.116176. Epub 2024 Apr 23.

DOI:10.1016/j.jpba.2024.116176
PMID:38701535
Abstract

Pesticides play an important role in forensic toxicology and are usually classified as a single class of chemicals. Despite their commonly perceived unity, pesticides encompass a spectrum of compounds, including organophosphates, carbamates, pyrethroids or organochlorines, among others, each with varying degrees of toxicity. Pesticide analysis in post-mortem samples can be difficult due to the complexity of the samples and to the high toxicity of these compounds. The aim of this study was to develop and validate an easy to use, sensitive, and robust method, using ultra-performance liquid chromatography-tandem mass spectrometry to be incorporated in the routine flow for pesticide analysis in post-mortem blood samples. Described herein is a streamlined, expeditious, yet highly efficient method facilitating the screening, qualitative assessment, and quantitative confirmation of 15 pesticides, including acetamiprid, azinphos-ethyl, bendiocarb, carbofuran, chlorfenvinphos, dimethoate, imidaclopride, malathion, methiocarb, methomyl, parathion, pirimicarb, strychnine, tetrachlorvinphos, and thiacloprid in post-mortem blood, recognizing the pivotal role blood plays in forensic investigations. The developed method was linear from 10 to 200 ng/mL; limits of detection were between 1 and 10 ng/mL, depending on the compound; it was successfully evaluated a dilution ratio of 1-2, 5 and 10; and 8 substances showed maximum stability for the time interval studied. This UHPLC-MS/MS method is useful and a powerful tool in a toxicology lab because it is fast, simple, effective, and trustworthy. The results of this validation highlight the robustness of the analytical method, providing a valuable tool for the accurate and sensitive detection of pesticides in post-mortem blood. Poised for routine implementation, this method has already found success in suspected intoxication cases, promising to elevate the standards of forensic pesticide analysis.

摘要

农药在法医毒理学中起着重要作用,通常被归类为单一类别的化学物质。尽管它们通常被认为是统一的,但农药包含一系列化合物,包括有机磷、氨基甲酸酯、拟除虫菊酯或有机氯等,每种化合物的毒性都不同。由于样品的复杂性和这些化合物的高毒性,死后样品中的农药分析可能很困难。本研究旨在开发和验证一种易于使用、灵敏且强大的方法,使用超高效液相色谱-串联质谱法纳入死后血液样品中农药分析的常规流程。本文介绍了一种简化、快速但高效的方法,用于筛选、定性评估和定量确认 15 种农药,包括乙酰甲胺磷、敌百虫、苯硫威、克百威、氯氟磷、乐果、氯吡虫啉、马拉硫磷、涕灭威、灭多威、对硫磷、嘧啶、西维因、毒杀芬和噻虫啉,这些农药存在于死后血液中,认识到血液在法医调查中的关键作用。所开发的方法在 10 至 200ng/mL 范围内呈线性;检测限取决于化合物,在 1 至 10ng/mL 之间;成功评估了 1:2、5 和 10 的稀释比;在研究的时间间隔内,有 8 种物质显示出最大的稳定性。这种 UHPLC-MS/MS 方法在毒理学实验室中是有用且强大的工具,因为它快速、简单、有效且可靠。该验证结果突出了分析方法的稳健性,为准确、灵敏地检测死后血液中的农药提供了有价值的工具。这种方法已经在疑似中毒病例中取得了成功,有望提高法医农药分析的标准,准备常规实施。

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