Simultaneous determination of mycotoxins and pesticides by UHPLC-HRMS in aquaculture feed from intensive farms

  • Acknowledgements: JMS thanks the University of Almería for his “Convocatoria de Recualificación del Sistema Universitario Español-Margarita Salas” postdoc grant under the “Plan de Recuperación Transformación” program funded by the Spanish Ministry of Universities with European Union's NextGenerationEU funds. RLR acknowledges the Andalusian Ministry of Economic Transformation, Industry, Knowledge and Universities for financial support from “Ayudas para Captación, Incorporación y Movilidad de Capital Humano de I+D+i (PAIDI 2020)”. MHM gratefully acknowledges the grant RYC2023-044255-I funded by MCIU/AEI/10.13039/501100011033 and FSE+. MAR gratefully acknowledges the contract from the project PROYEXCEL_00195, funded by Consejería de Universidad, Investigación e Innovación, Junta de Andalucía. This research was also funded by Project PID2021-1278040BI00 funded by Spanish MCIN/ AEI /10.13039/501100011033 and by “ERDF A way of making Europe”, Spanish MCIU-FEDER (grant # PID2021-122287OB-C21), CEIMAR and LifeBioencapsulation S.L. UAL- spin-off (grant #CEIJ-C05.1-2019).
  • Authors: J. Marín-Sáez, M. Álvarez-Romero, R. López-Ruiz, A.M. García-Campaña, Mª.I. Sáez, L. Gámiz-Gracia, A. Garrido Frenich, Maykel Hernández-Mesa.
  • Reference: Microchemical Journal 219 (2025) 11604.

Background: Intensive aquaculture in southern Spain is growing, leading to increased use of plant-based in- gredients in fish feed. While this shift results in more nutritionally balanced feeds, it also introduces the risk of contaminants like mycotoxins and pesticides, which can negatively affect feed production, fish health, and pose potential risks to consumers. However, studies on these contaminants in aquaculture feed are limited. Results: In this study, a multiclass method was developed to determine 27 mycotoxins and 11 pesticides in aquaculture feed by ultrahigh performance liquid chromatography coupled with high resolution mass spec- trometry (UHPLC-HRMS). The method involved a previous ultrasound-assisted solid-liquid extraction using an acidified mixture of acetonitrile and water, followed by a dispersive solid-phase extraction with MgSO4 and C18. Characterization of the method was satisfactory for almost all compounds, with recovery values between 70 and 120 % and relative standard deviations (RSDs) below 20 %. The quantification limits were comparable to those reported in studies focusing on a single family of compounds. The method was applied to the analysis of aquaculture feeds with diverse compositions, revealing a high incidence of the mycotoxins enniatins, as well as the pesticides tebuconazole and pirimiphos methyl. Conclusion: The possible source of these contaminants and residues was investigated by analysing the main raw materials of the feeds, attempting to link their origin with the wheat and soy. Additionally, non-targeted analysis identified six additional pesticides, and one pesticide adjuvant not included in the targeted analysis, highlighting the importance of such studies.

This entry was posted in Animal feed, Mass spectrometry, Mycotoxins, PID2021-127804OB-I00, PROYEXCEL_00195, Pesticides, RYC2023-044255-I, UHPLC, USLE, dSPE and tagged , , , . Bookmark the permalink.