Assessing human exposure to pesticides and mycotoxins: optimization and validation of a method for multianalyte determination in urine samples.

  • Acknowledgements: Funding for open access publishing: Universidad de Almería/CBUA. This work was supported by Andalusian Government (Project ref. PROYEXCEL_00195) and PID2021-127804OB-I00 funded by Spanish MCIN/AEI/ 10.13039/501100011033 and by “ERDF A way of making Europe”. JMS thanks the University of Almería for his “Convocatoria de Recualificación do Sistema Universitario Español-Margarita Salas” postdoc grant under the “Plan de Recuperación Transformación” programme funded by the Spanish Ministry of Universities with European Union’s NextGenerationEU funds. MHM gratefully acknowledges the grant IJC2019-040989-I funded by MCIN/AEI/ 10.13039/501100011033.
  • Authors: J. Marín-Sáez, M. Hernández-Mesa, J.A. Gallardo-Ramos, L. Gámiz-Gracia, A.M. García-Campaña.
  • Reference: Analytical and Bioanalytical Chemistry 416 (2024) 1935–1949.

Humans are exposed to an increasing number of contaminants, with diet being one of the most important exposure routes. In this framework, human biomonitoring is considered the gold standard for evaluating human exposure to chemicals. Pesticides and mycotoxins are chemicals of special concern due to their health implications. They constitute the predominant border rejection notifications for food and feed in Europe and the USA. However, current biomonitoring studies are focused on a limited number of compounds and do not evaluate mycotoxins and pesticides together. In this study, an analytical method has been developed for the determination of 30 pesticides and 23 mycotoxins of concern in urine samples. A salting-out liquid–liquid extraction (SALLE) procedure was optimized achieving recoveries between 70 and 120% for almost all the compounds and limits as lower as when QuEChERS was applied. The compounds were then determined by liquid chromatography coupled to triple quadrupole mass spectrometry. Different chromatographic conditions and analytical columns were tested, selecting a Hypersild gold aQ column as the best option. Finally, the method was applied to the analysis of 45 urine samples, in which organophosphate and pyrethroid pesticides (detection rates (DR) of 82% and 42%, respectively) and ochratoxin A and deoxynivalenol (DR of 51% and 33%, respectively) were the most detected compounds. The proposed analytical method involves the simultaneous determination of a diverse set of pesticides and mycotoxins, including their most relevant metabolites, in human urine. It serves as an essential tool for biomonitoring the presence of highly prevalent contaminants in modern society.

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