title: LC/DAD/ESI/MS method for the determination of imidacloprid, thiacloprid, and spinosad in olives and olive oil after field treatment.
abstract: The behavior in the field and the transfer from olives to olive oil during the technological process of imidacloprid, thiacloprid, and spinosad were studied. The extraction method used was effective in extracting the analytes of interest, and no interfering peaks were detected in the chromatogram. The residue levels found in olives after treatment were 0.14, 0.04, and 0.30 mg/kg for imidacloprid, thiacloprid, and spinosad, respectively, far below the maximum residue levels (MRLs) set for these insecticides in EU. At the preharvest interval (PHI), no residue was detected for imidacloprid and thiacloprid, while spinosad showed a residue level of 0.04 mg/kg. The study of the effect of the technological process on pesticide transfer in olive oil showed that these insecticides tend to remain in the olive cake. The LC/DAD/ESI/MS method showed good performance with adequate recoveries ranging from 80 to 119% and good method limits of quantitation (LOQs) and of determination (LODs). No matrix effect was detected.
authors.affiliation: Department of Pharmaceutical Chemistry and Technology, Università degli Studi di Cagliari, via Ospedale 72, 09124 Cagliari, Italy. aangioni@unica.it
authors.forename: Alberto
authors.initials: A
authors.lastname: Angioni
authors.forename: Luciano
authors.initials: L
authors.lastname: Porcu
authors.forename: Filippo
authors.initials: F
authors.lastname: Pirisi
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004338:Drug Combinations; D005506:Food Contamination / Q000032:analysis; D005638:Fruit / Q000737:chemistry; D007093:Imidazoles / Q000032:analysis; D007306:Insecticides / Q000032:analysis*; D018942:Macrolides / Q000032:analysis; D000073943:Neonicotinoids; D009574:Nitro Compounds / Q000032:analysis; D031658:Olea / Q000737:chemistry*; D000069463:Olive Oil; D010573:Pesticide Residues / Q000032:analysis; D010938:Plant Oils / Q000737:chemistry*; D011725:Pyridines / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013843:Thiazines / Q000032:analysis
chemical_list: D004338:Drug Combinations; D007093:Imidazoles; D007306:Insecticides; D018942:Macrolides; D000073943:Neonicotinoids; D009574:Nitro Compounds; D000069463:Olive Oil; D010573:Pesticide Residues; D010938:Plant Oils; D011725:Pyridines; D013843:Thiazines; C082359:imidacloprid; C417209:thiacloprid; C415329:spinosad