title: Micro-solid-phase extraction (µ-SPE) of organophosphorous pesticides from wheat followed by LC-MS/MS determination.
abstract: A rapid, selective and effective method of extraction, clean-up and concentration of organophosphorous pesticides from wheat followed by electrospray (ESI) LC-MS/MS analysis was developed. The μ-SPE (micro-solid-phase extraction) procedure resulted in good analytical performance and reduced at the same time matrix effects, analysis time and solvent consumption. Limits of detection (LODs) and quantification (LOQs) were in the range of 0.3-10 and 1-30 μg kg(-1), respectively, with good reproducibility (RSD ≤ 13.8) and recoveries between 75% and 109%. Coefficients of determination (r(2)) were greater than 0.996 for the studied pesticides. Despite the reduced sorbent bed mass of μ-SPE tips (4.2 mg), the analytical data showed that no saturation phenomena occurs in the tested range of concentration both for single compounds and mixtures. Several real samples were analysed and the concentrations of the selected pesticides were found to be below the respective maximum residue limit (MRLs).
authors.affiliation: a Faculty of Bioscience and Technology for Food, Agriculture and Environment , University of Teramo , Teramo , Italy.
authors.forename: Flavio
authors.initials: F
authors.lastname: Della Pelle
authors.affiliation: a Faculty of Bioscience and Technology for Food, Agriculture and Environment , University of Teramo , Teramo , Italy.
authors.forename: Maria Chiara
authors.initials: MC
authors.lastname: Di Crescenzo
authors.affiliation: a Faculty of Bioscience and Technology for Food, Agriculture and Environment , University of Teramo , Teramo , Italy.
authors.forename: Manuel
authors.initials: M
authors.lastname: Sergi
authors.affiliation: b Department of Chemistry , Sapienza University of Rome , Rome , Italy.
authors.forename: Camilla
authors.initials: C
authors.lastname: Montesano
authors.affiliation: a Faculty of Bioscience and Technology for Food, Agriculture and Environment , University of Teramo , Teramo , Italy.|b Department of Chemistry , Sapienza University of Rome , Rome , Italy.
authors.forename: Francesca
authors.initials: F
authors.lastname: Di Ottavio
authors.affiliation: c Istituto Zooprofilattico Sperimentale dell'Abruzzo e del Molise 'G. Caporale' , Teramo , Italy.
authors.forename: Rossana
authors.initials: R
authors.lastname: Scarpone
authors.affiliation: c Istituto Zooprofilattico Sperimentale dell'Abruzzo e del Molise 'G. Caporale' , Teramo , Italy.
authors.forename: Giampiero
authors.initials: G
authors.lastname: Scortichini
authors.affiliation: a Faculty of Bioscience and Technology for Food, Agriculture and Environment , University of Teramo , Teramo , Italy.
authors.forename: Dario
authors.initials: D
authors.lastname: Compagnone
mesh_terms: D002853:Chromatography, Liquid; D005504:Food Analysis; D005506:Food Contamination / Q000032:analysis*; D009943:Organophosphorus Compounds / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D014908:Triticum / Q000737:chemistry*
chemical_list: D009943:Organophosphorus Compounds; D010575:Pesticides
keywords: LC-MS/MS; Organophosphrous pesticides; micro-solid-phase extraction (µ-SPE); wheat