Pérez Figueroa, J. L.Fernández Hernando, PilarGarcía Mayor, M AsunciónGarcinuño Martínez, Rosa Mª2026-01-162026-01-162025-10-07Pérez-Figueroa, Fernández-Hernando, Mayor, M. A. G., & Garcinuño. (2025). New salty extraction of polar analytes technique and oil-based cleanup (SExPA-Oc) for the determination of nereistoxins in vegetable samples with HILIC-MS/MS. Food Chemistry, 496. https://doi.org/10.1016/j.foodchem.2025.1466680308-8146https://doi.org/10.1016/j.foodchem.2025.146668https://hdl.handle.net/20.500.14468/31433The registered version of this article, first published in “Food Chemistry, 496, 146668", is available online at the publisher's website: https://doi.org/10.1016/j.foodchem.2025.146668La versión registrada de este artículo, publicado por primera vez en “Food Chemistry, 496, 146668", está disponible en línea en el sitio web del editor: https://doi.org/10.1016/j.foodchem.2025.146668Nereistoxins are polar, unstable insecticides that present significant analytical challenges in agricultural products due to rapid degradation, limiting reliable monitoring in food safety programs. This study was carried out to address these challenges by developing a stable, efficient, and cost-effective method for the extraction and quantification of nereistoxins (cartap, nereistoxin, thiocyclam, thiosultap) in tomatoes, avocados, and olive oil. The novel SExPA-Oc (salty extraction of polar analytes–oil cleanup) method uses a salt-assisted liquid-liquid partition combined with an olive oil cleanup step, eliminating the need for expensive sorbents while improving analyte stability. Analysis by Hydrophilic Interaction Liquid Chromatography coupled with tandem mass spectrometry (HILIC-MS) achieved a linear range of 3–800 μg/kg and recoveries exceeding 70 % in most matrices, with limits of quantification meeting regulatory standards. This strategy provides a robust, environmentally friendly solution for nereistoxin analysis, addressing gaps in food safety monitoring and broader applicability to other polar, unstable compounds.eninfo:eu-repo/semantics/openAccess2301 Química analíticaartículoAgrochemical residuesFood safety monitoringLiquid-liquid extractionOlive oil cleanup