Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, Friedrich-Alexander-Universität Erlangen-Nürnberg, Germany.
Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, Friedrich-Alexander-Universität Erlangen-Nürnberg, Germany.
Toxicol Lett. 2018 Dec 1;298:33-41. doi: 10.1016/j.toxlet.2018.07.048. Epub 2018 Jul 30.
Organophosphate pesticides (OPP) and carbamates are still counted among the most prominent agents used for crops protection. Up to date the determination of dialkylphosphates and their thio derivatives in urine is established for the OPP biomonitoring. However, this approach does not provide information on the exposure to specific OPP agents. A lot of OPP as well as some carbamates also provide specific urinary biomarkers indeed. Analytical methods for the determination of phenolic metabolites of OPP and carbamates have already been established by different working groups. However, these approaches only acquire one or few analytes. Therefore, we developed an analytical procedure which enables the simultaneous assessment of a wide spectrum of phenolic metabolites of OPP, carbamates and other pesticides in human urine using GC-MS/MS. The method includes enzymatic hydrolysis, solid phase extraction, derivatization, and subsequent GC-MS/MS analysis. The method showed detection limits between 0.1 and 0.4 μg/l. Variation coefficients ranged from 1 to 9 % for precision in series and 1 % to 13 % for inter-day precision. Furthermore, recovery rates between 87 and 117 % were determined. Compared with other published analytical procedures, the present method enables the simultaneous monitoring of a much broader spectrum of pesticides and biocides whose structures contain aryl moieties with competitive or improved analytical reliability. Furthermore, the suitability of the developed procedure was verified through the successful application to urine samples of pesticide exposed humans.
有机磷农药（OPP）和氨基甲酸酯类农药仍然被认为是用于作物保护的最主要的药剂之一。迄今为止，用于 OPP 生物监测的方法是测定尿液中的二烷基磷酸酯及其硫代衍生物。然而，这种方法并不能提供关于接触特定 OPP 药剂的信息。实际上，许多 OPP 以及一些氨基甲酸酯类农药也提供了特定的尿液生物标志物。不同的研究小组已经建立了用于测定 OPP 和氨基甲酸酯类酚代谢物的分析方法。然而，这些方法只能获取一种或几种分析物。因此，我们开发了一种分析程序，可以使用 GC-MS/MS 同时评估人类尿液中 OPP、氨基甲酸酯类和其他农药的广泛酚代谢物。该方法包括酶水解、固相萃取、衍生化和随后的 GC-MS/MS 分析。该方法的检测限在 0.1 至 0.4μg/l 之间。精密度的变异系数在 1%至 9%之间，日间精密度的变异系数在 1%至 13%之间。此外，回收率在 87%至 117%之间。与其他已发表的分析方法相比，本方法能够同时监测结构中含有芳基部分的更广泛的农药和杀生物剂，具有竞争或改进的分析可靠性。此外，通过成功应用于暴露于农药的人类尿液样本，验证了所开发程序的适用性。
