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