This study presents a novel sample preparation method for the determination of both specific and non-specific pesticide metabolites in human urine samples. The method combines a deconjugation step with QuEChERS-based method and solid-phase extraction. In total, 15 pesticide metabolites (diethyl phosphate; diethyl thiophosphate; dimethyl phosphate; diethyl thiophosphate; 2,4-dichlorophenoxyacetic acid; 3-phenoxybenzoic acid; 4-fluoro-3-phenoxybenzoic acid; coumaphos; diethyl dithiophosphate; malathion dicarboxylic acid; p-nitrophenol; cis/trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane carboxylic acid; 3,5,6-trichloro-2-pyridinol; N,N-diethyl-3-methylbenzamid and 2-isopropyl-4-methyl-6-hydroxypyrimidine) were separated using liquid chromatography coupled to a mass spectrometer and isotope dilution method for quantitation. The method was validated using recovery tests with recoveries generally ranging from 80 to 120%. Additionally, 20 urine samples collected from South African children were analysed using the presented method. The median levels of pesticide metabolites found in the urine samples ranged from not detected (N,N-diethyl-3-methylbenzamid) to 22.36 µg/g creatinine (dimethyl phosphate). The novel method developed in this study is sensitive, selective, robust and reproducible while also conserving the amount of sample, chemicals, material and time required. Due to the low limits of detection obtained for individual pesticide metabolites, the method is capable of quantifying trace levels of pesticide metabolites in urine, which thus makes it an ideal tool for biomonitoring studies.

这项研究提出了一种测定人尿液样品中特定和非特定农药代谢物的新型样品制备方法。该方法将解偶联步骤与基于QuEChERS的方法和固相萃取相结合。总共有15种农药代谢物（磷酸二乙酯;硫代磷酸二乙酯;磷酸二甲酯;硫代磷酸二乙酯; 2,4-二氯苯氧基乙酸; 3-苯氧基苯甲酸; 4-氟-3-苯氧基苯甲酸;香豆磷;二乙基二硫代磷酸盐;马拉硫磷二羧酸; p -硝基苯酚;顺/反-3-（2,2-二氯乙烯基）-2,2-二甲基环丙烷甲酸; 3,5,6-三氯-2-吡啶醇; N，N（1-二乙基-3-甲基苯甲酰胺和2-异丙基-4-甲基-6-羟基嘧啶）使用与质谱仪偶联的液相色谱法和同位素稀释法进行分离。使用回收率测试验证了该方法，回收率通常为80％至120％。另外，使用提出的方法分析了从南非儿童收集的20个尿液样本。在尿液样本中发现的农药代谢物的中位数水平范围为未检测到（N，N-二乙基-3-甲基苯甲酰胺）至22.36 µg / g肌酐（磷酸二甲酯）。本研究开发的新方法灵敏，选择性强，可重现，同时还节省了所需的样品量，化学药品，材料和时间。由于对单个农药代谢物的检测限较低，因此该方法能够定量尿液中痕量农药代谢物的含量，因此使其成为生物监测研究的理想工具。