title: Determination of polar pesticides in olive oil and olives by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry and high resolution mass spectrometry.
abstract: This article reports the development of two HPLC-MS methods for the determination of polar pesticides in olive oil and olive samples by hydrophilic interaction liquid chromatography (HILIC) separation followed by mass spectrometry detection with tandem mass spectrometry using a triple quadrupole instrument operated in multiple reaction monitoring mode (HILIC-MS/MS) or electrospray time-of-flight mass spectrometry (HILIC-TOFMS). The selected polar pesticides included in the study were: amitrol, cyromazine, diquat, paraquat, mepiquat, trimethylsulfonium (trimesium, glyphosate counterion) and fosetyl aluminium. The simple sample treatment procedure was based on liquid partitioning with methanol. The performance of the sample extraction was evaluated in terms of recovery rates and matrix effects in both olive oil and olives matrices. The results obtained for olive oil were satisfactory while, due to the high complexity of olives, poor recovery rates were obtained for the extraction of diquat, paraquat and amitrol, although with a reasonable precision enabling its use in routine analysis. Similarly, matrix effects were minor in the case of olive oil (ca. 20% suppression average), while significantly higher suppression was observed for olives (30-50% suppression average). The studied approaches were found to be useful for the determination of the pesticides studied in olive oil and olives with limits of quantitation below 5µgkg(-1) in most cases when tandem mass spectrometry was used, thus being in compliance with MRLs set by current EU regulation.
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071 Jaén, Spain.
authors.forename: Rocío
authors.initials: R
authors.lastname: Nortes-Méndez
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071 Jaén, Spain.
authors.forename: José
authors.initials: J
authors.lastname: Robles-Molina
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071 Jaén, Spain.
authors.forename: Rafael
authors.initials: R
authors.lastname: López-Blanco
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071 Jaén, Spain; Department of Applied Chemistry, Faculty of Food Science, Szent István University, Villányi út 29-43, H-1118 Budapest, Hungary.
authors.forename: Andrea
authors.initials: A
authors.lastname: Vass
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071 Jaén, Spain; Center for Advanced Studies in Olives Grove and Olive Oils (CEAOAO), Science and Technology Park GEOLIT, E-23620 Mengíbar, Spain.
authors.forename: Antonio
authors.initials: A
authors.lastname: Molina-Díaz
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edif. B-3, 23071 Jaén, Spain. Electronic address: jfgreyes@ujaen.es.
authors.forename: Juan F
authors.initials: JF
authors.lastname: Garcia-Reyes
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D005506:Food Contamination / Q000032:analysis*; D005638:Fruit / Q000737:chemistry*; D057927:Hydrophobic and Hydrophilic Interactions; D013058:Mass Spectrometry / Q000379:methods; D031658:Olea; D000069463:Olive Oil / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis*
chemical_list: D000069463:Olive Oil; D010573:Pesticide Residues
keywords: HILIC; Liquid chromatography/mass spectrometry (LC–MS); Olive oil; Olives; Polar pesticides