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Large multiresidue analysis of pesticides in edible vegetable oils by using efficient solid-phase extraction sorbents based on quick, easy, cheap, effective, rugged and safe methodology followed by gas chromatography-tandem mass spectrometry.

P. Parrilla Vázquez, E. Hakme, S. Uclés, V. Cutillas, M. Martínez Galera, A.R. Mughari, Amadeo R. Fernández-Alba

European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables (EURL-FV), University of Almeria, Agrifood Campus of InternationalExcellence (ceiA3), Almeria, Spain

Journal of Chromatography A, 1463 (2016) 20–31



The aim of this research was to adapt the QuEChERS method for routine pesticide multiresidue anal-ysis in edible vegetable oil samples using gas chromatography coupled to tandem mass spectrometry(GC–MS/MS). Several clean-up approaches were tested: (a) D-SPE with Enhanced Matrix Removal-Lipid(EMR-LipidTM); (b) D-SPE with PSA; (c) D-SPE with Z-Sep; (d) SPE with Z-Sep. Clean-up methods wereevaluated in terms of fat removal from the extracts, recoveries and extraction precision for 213 pesticidesin different matrices (soybean, sunflower and extra-virgin olive oil). The QuEChERS protocol with EMR-Lipid d-SPE provided the best reduction of co-extracted matrix compounds with the highest number ofpesticides exhibiting mean recoveries in the 70–120% range, and the lowest relative standard deviationsvalues (4% on average). A simple and rapid (only 5 min) freeze-out step with dry ice (CO2at −76◦C) priorto d-SPE clean-up ensured much better removal of co-extracted matrix compounds in compliance of thenecessity in routine analysis. Procedural Standard Calibration was established in order to compensate forrecovery losses of certain pesticides and possible matrix effects. Limits of quantification were 10 g kg−1for the majority of the pesticides. The modified methodology was applied for the analysis of different17 oil samples. Fourteen pesticides were detected with values lower than MRLs and their concentrationranged between 10.2 and 156.0 g kg−1.

© 2016 Elsevier B.V. All rights reserved.


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Published 08-02-2017, 16:33:50

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