title: Rapid determination of residues of pesticides in honey by µGC-ECD and GC-MS/MS: Method validation and estimation of measurement uncertainty according to document No. SANCO/12571/2013.
abstract: A simple and straightforward method for simultaneous determination of residues of 13 pesticides in honey samples (acrinathrin, bifenthrin, bromopropylate, cyhalothrin-lambda, cypermethrin, chlorfenvinphos, chlorpyrifos, coumaphos, deltamethrin, fluvalinate-tau, malathion, permethrin and tetradifon) from different pesticide classes has been developed and validated. The analytical method provides dissolution of honey in water and an extraction of pesticide residues by n-Hexane followed by clean-up on a Florisil SPE column. The extract was evaporated and taken up by a solution of an injection internal standard (I-IS), ethion, and finally analyzed by capillary gas chromatography with electron capture detection (GC-µECD). Identification for qualitative purpose was conducted by gas chromatography with triple quadrupole mass spectrometer (GC-MS/MS). A matrix-matched calibration curve was performed for quantitative purposes by plotting the area ratio (analyte/I-IS) against concentration using a GC-µECD instrument. According to document No. SANCO/12571/2013, the method was validated by testing the following parameters: linearity, matrix effect, specificity, precision, trueness (bias) and measurement uncertainty. The analytical process was validated analyzing blank honey samples spiked at levels equal to and greater than 0.010 mg/kg (limit of quantification). All parameters were satisfactorily compared with the values established by document No. SANCO/12571/2013. The analytical performance was verified by participating in eight multi-residue proficiency tests organized by BIPEA, obtaining satisfactory z-scores in all 70 determinations. Measurement uncertainty was estimated according to the top-down approaches described in Appendix C of the SANCO document using the within-laboratory reproducibility relative standard deviation combined with laboratory bias using the proficiency test data.
authors.affiliation: a Environmental Contaminants Laboratory, Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche , Perugia , Italy.
authors.forename: Angela
authors.initials: A
authors.lastname: Paoloni
authors.affiliation: a Environmental Contaminants Laboratory, Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche , Perugia , Italy.
authors.forename: Sabrina
authors.initials: S
authors.lastname: Alunni
authors.affiliation: a Environmental Contaminants Laboratory, Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche , Perugia , Italy.
authors.forename: Alessandro
authors.initials: A
authors.lastname: Pelliccia
authors.affiliation: a Environmental Contaminants Laboratory, Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche , Perugia , Italy.
authors.forename: Ivan
authors.initials: I
authors.lastname: Pecorelli
mesh_terms: D002138:Calibration; D005062:European Union; D005504:Food Analysis / Q000379:methods / Q000592:standards / Q000706:statistics & numerical data; D005506:Food Contamination / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006586:Hexanes / Q000737:chemistry; D006722:Honey / Q000032:analysis*; D057230:Limit of Detection; D010573:Pesticide Residues / Q000032:analysis; D010575:Pesticides / Q000032:analysis* / Q000737:chemistry; D053719:Tandem Mass Spectrometry; D035501:Uncertainty
chemical_list: D006586:Hexanes; D010573:Pesticide Residues; D010575:Pesticides; C026385:n-hexane
keywords: SANCO 12571/2013; Uncertainty estimation; honey; pesticide residues; top-down approach