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采用液相色谱-串联三重四极杆质谱法同时测定人血清中的极性农药。

Simultaneous determination of polar pesticides in human blood serum by liquid chromatography coupled to triple quadrupole mass spectrometer.

机构信息

Research Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics, Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), University of Almeria, Agrifood Campus of International Excellence, ceiA3, E-04120, Almeria, Spain.

Research Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics, Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), University of Almeria, Agrifood Campus of International Excellence, ceiA3, E-04120, Almeria, Spain.

出版信息

J Pharm Biomed Anal. 2020 Oct 25;190:113492. doi: 10.1016/j.jpba.2020.113492. Epub 2020 Jul 25.

Abstract

In this study a simple and rapid method was used for the determination of 5 polar pesticides and 3 metabolites, ethephon, 2-hydroxyethyl phosphonic acid (HEPA), fosetyl-aluminum, phosphonic acid, glyphosate, chlorate, glufosinate and 3-methylphosphinicopropionic acid (MPPA) in human blood serum. Acidified water (1% formic acid) and acetonitrile (1% formic acid) were used as extraction solvents and n-hexane was utilized as a clean-up step for lipid removal. The analytical method was based on liquid chromatography coupled to triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS). The proposed method was validated, obtaining recoveries ranging from 70 to 110% and precision values lower than 17% for all analytes. Limit of quantification was 0.01 mg/L for ethephon, fosetyl-aluminum, MPPA and HEPA, 0.025 mg/L for glyphosate, phosphonic acid and chlorate and 0.05 mg/L for glufosinate. This is the first time that an analytical method was developed for the determination of a high number of polar pesticides in human blood serum, allowing the simultaneous monitoring of these compounds in a complex matrix as human blood serum.

摘要

在这项研究中,采用了一种简单快速的方法来测定人血清中的 5 种极性农药和 3 种代谢物,即乙烯利、2-羟乙基膦酸(HEPA)、福赛膦、膦酸、草甘膦、氯酸盐、草铵膦和 3-甲基膦酸丙酯(MPPA)。酸化水(1%甲酸)和乙腈(1%甲酸)被用作提取溶剂,正己烷被用作去除脂质的净化步骤。分析方法基于液相色谱-串联三重四极杆质谱(LC-QqQ-MS/MS)。该方法经过验证,所有分析物的回收率在 70%至 110%之间,精密度值低于 17%。乙磷、福赛膦、MPPA 和 HEPA 的定量限为 0.01mg/L,草甘膦、膦酸和氯酸盐的定量限为 0.025mg/L,草铵膦的定量限为 0.05mg/L。这是首次开发出用于测定人血清中大量极性农药的分析方法,允许在人血清等复杂基质中同时监测这些化合物。

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