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通过液质联用(LC-ESI-MS-MS)技术测定法医案例血液中的涕灭威、克百威和甲胺磷。

Determination of Aldicarb, Carbofuran and Methamidophos in Blood Derived from Forensic Cases through Liquid Chromatography with Electrospray Ionization and Tandem Mass Spectrometry (LC--ESI-MS-MS).

机构信息

Toxicology Laboratory of the National Institute of Legal Medicine and Forensic Sciences, Bogotá 110321, Colombia.

Department of Toxicology, Universidad Nacional de Colombia, Bogotá 111321, Colombia.

出版信息

J Anal Toxicol. 2022 Feb 14;46(1):37-46. doi: 10.1093/jat/bkaa182.

DOI:10.1093/jat/bkaa182
PMID:33258956
Abstract

The presence and use of carbamate and organophosphate pesticides with agricultural and urban purposes in Colombia has been justified for pest control. However, these substances pose a national problem because of their toxic nature, which is associated with accidental poisoning or even with homicides or suicides related to acute fatal poisoning. This study aims to develop and to validate an analytical methodology for the determination of the aldicarb, carbofuran and methamidophos pesticides in blood through liquid chromatography--tandem mass spectrometry (LC-MS-MS). To this end, the method for extracting pesticides from the blood was developed, the conditions of LC were defined, the instrumental system MS-MS was optimized and the bioanalytical methodology was validated. This methodology proved to be selective, precise, accurate and linear in the concentration range from 0.10 to 5.0 µg/mL, with a limit of detection of 0.020 µg/mL for aldicarb and carbofuran and 0.050 µg/mL for methamidophos, recovery between 90% and 102%, and stability at room temperature and in the autosampler between 80% and 120%. The analytical methodology was applied to 34 forensic cases. Carbofuran was found at a concentration ranging from 0.020 to >5.0 µg/mL, aldicarb was found at a concentration ranging from 0.10 to 2.5 µg/mL and methamidophos was found at a concentration >5.0 µg/mL. In 62% of the cases, the pesticides under study were used to commit suicide. Necropsy findings of pesticide poisoning are non-specific. Therefore, toxicological blood analysis provides significant information at the forensic level, and the analytical method validated represents a sensitive, fast and reliable analysis with little solvent consumption of a small sample amount, so it is suitable for routine application in fatal pesticide poisonings.

摘要

哥伦比亚存在并使用具有农业和城市用途的氨基甲酸酯和有机磷农药来控制虫害,这是有其合理性的。然而,由于这些物质具有毒性,这给国家带来了一个问题,因为它们与意外中毒甚至与与急性致命中毒有关的凶杀或自杀有关。本研究旨在开发和验证一种通过液相色谱-串联质谱(LC-MS-MS)测定血液中涕灭威、克百威和甲胺磷农药的分析方法。为此,开发了从血液中提取农药的方法,定义了 LC 条件,优化了仪器系统 MS-MS,并验证了生物分析方法。该方法在 0.10 至 5.0 µg/mL 的浓度范围内表现出选择性、精确性、准确性和线性,涕灭威和克百威的检测限为 0.020 µg/mL,甲胺磷的检测限为 0.050 µg/mL,回收率在 90%至 102%之间,在室温下和自动进样器中在 80%至 120%之间稳定。该分析方法应用于 34 例法医案例。检测到的克百威浓度范围为 0.020 至>5.0 µg/mL,涕灭威浓度范围为 0.10 至 2.5 µg/mL,甲胺磷浓度>5.0 µg/mL。在 62%的情况下,研究中的农药被用于自杀。农药中毒的尸检结果是非特异性的。因此,毒理学血液分析在法医层面提供了重要信息,所验证的分析方法代表了一种灵敏、快速和可靠的分析方法,溶剂消耗少,对小样本量进行分析,因此适合常规应用于致命农药中毒。

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