title: Validation and application of micro flow liquid chromatography-tandem mass spectrometry for the determination of pesticide residues in fruit jams.
abstract: In this study, a very sensitive method was validated to determine pesticides residues in fruit jams using micro flow liquid chromatography-tandem mass spectrometry (µLC-MS/MS). A slurry of the fruit jams and water was prepared to yield homogeneous samples. Because of the high sensitivity achieved with the µLC-MS/MS equipment and to minimize matrix effects, the QuEChERS extracts were diluted 30-fold before the analysis. The validation was performed analyzing spiked samples at 9 and 45 µg kg(-1) (n=5). The method met validation criteria of 70-120% recovery and RSD≤20% for 92% of the 107 pesticides evaluated. The reporting limit (RL) was 9 and 45 µg kg(-1) for respectively 66% and 26% of the analytes, 5% of the compounds did not fulfill the requirements for validation and 3% were not detected at the studied concentrations. The validated method was applied to the analysis of 51 different fruit jam samples from Brazil and Spain and pesticide residues were detected in 41 samples, 26 of which contained at least one pesticide at concentration >10 µg kg(-1).
authors.affiliation: Department of Food Science and Technology, Federal University of Santa Maria (UFSM), Roraima 1000/42, 97105-900 Santa Maria, RS, Brazil; CAPES Foundation, Ministry of Education of Brazil, Brasília-DF 70040-020, Brazil.
authors.forename: Bárbara
authors.initials: B
authors.lastname: Reichert
authors.affiliation: Federal University of Santa Maria, Chemistry Department, Center of Research and Analysis of Residues and Contaminants (CEPARC), Santa Maria, RS, Brazil.
authors.forename: Ionara Regina
authors.initials: IR
authors.lastname: Pizzutti
authors.affiliation: Department of Morphology, Federal University of Santa Maria (UFSM), Roraima 1000/19, 97105-900 Santa Maria, RS, Brazil.
authors.forename: Ijoni Hilda
authors.initials: IH
authors.lastname: Costabeber
authors.affiliation: European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, University of Almeria, Agrifood Campus of International Excellence (ceiA3), Agrifood, Spain.
authors.forename: Ana
authors.initials: A
authors.lastname: Uclés
authors.affiliation: European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, University of Almeria, Agrifood Campus of International Excellence (ceiA3), Agrifood, Spain.
authors.forename: Sonia
authors.initials: S
authors.lastname: Herrera
authors.affiliation: European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, University of Almeria, Agrifood Campus of International Excellence (ceiA3), Agrifood, Spain. Electronic address: amadeo@ual.es.
authors.forename: Amadeo R
authors.initials: AR
authors.lastname: Fernández-Alba
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods; D005506:Food Contamination / Q000032:analysis*; D057141:Food, Preserved / Q000032:analysis*; D005638:Fruit; D010573:Pesticide Residues / Q000032:analysis*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D010573:Pesticide Residues
keywords: Fruit jams; Pesticides residues determination; QuEChERS sample preparation; µLC–MS/MS