title: 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.
abstract: The aim of this research was to adapt the QuEChERS method for routine pesticide multiresidue analysis 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-Lipid™); (b) D-SPE with PSA; (c) D-SPE with Z-Sep; (d) SPE with Z-Sep. Clean-up methods were evaluated in terms of fat removal from the extracts, recoveries and extraction precision for 213 pesticides in 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 of pesticides exhibiting mean recoveries in the 70-120% range, and the lowest relative standard deviations values (4% on average). A simple and rapid (only 5min) freeze-out step with dry ice (CO2 at -76°C) prior to d-SPE clean-up ensured much better removal of co-extracted matrix compounds in compliance of the necessity in routine analysis. Procedural Standard Calibration was established in order to compensate for recovery losses of certain pesticides and possible matrix effects. Limits of quantification were 10μgkg(-1) for the majority of the pesticides. The modified methodology was applied for the analysis of different 17 oil samples. Fourteen pesticides were detected with values lower than MRLs and their concentration ranged between 10.2 and 156.0μgkg(-1).
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain.
authors.forename: P
authors.initials: P
authors.lastname: Parrilla Vázquez
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain.
authors.forename: E
authors.initials: E
authors.lastname: Hakme
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain.
authors.forename: S
authors.initials: S
authors.lastname: Uclés
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain.
authors.forename: V
authors.initials: V
authors.lastname: Cutillas
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain.
authors.forename: M
authors.initials: M
authors.lastname: Martínez Galera
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain.
authors.forename: A R
authors.initials: AR
authors.lastname: Mughari
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Cañada de San Urbano, 04120 Almería, Spain. Electronic address: amadeo@ual.es.
authors.forename: A R
authors.initials: AR
authors.lastname: Fernández-Alba
mesh_terms: D002138:Calibration; D002849:Chromatography, Gas; D000069463:Olive Oil / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis*; D010938:Plant Oils / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000191:economics / Q000379:methods*; D013024:Soybean Oil / Q000737:chemistry; D000074242:Sunflower Oil; D053719:Tandem Mass Spectrometry; D013997:Time Factors
chemical_list: D000069463:Olive Oil; D010573:Pesticide Residues; D010938:Plant Oils; D000074242:Sunflower Oil; D013024:Soybean Oil
keywords: EMR-Lipid; Edible vegetable oils; GC–MS/MS; Multiresidue pesticide analysis; Procedural Standard Calibration