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. Issue 3 (3rd March 2016)

• Record Type: Journal Article
• Authors: Paoloni, Angela; Alunni, Sabrina; Pelliccia, Alessandro; Pecorelli, Ivan
• Is Part Of: Journal of environmental science and health. Volume 51:Issue 3(2016)
• Page Start: 133
• Page End: 142
• Publication Date: 2016-03-03
• Subjects: Uncertainty estimation -- top-down approach -- honey -- SANCO 12571/2013 -- pesticide residues; Pesticides -- Environmental aspects -- Periodicals; Food contamination -- Periodicals; Agricultural wastes -- Environmental aspects -- Periodicals; Ecology -- periodicals; Pesticides -- toxicity -- periodicals; Food Contamination -- periodicals; 363.73
• DOI: 10.1080/03601234.2015.1108748
• Languages: English
• ISSNs: 0360-1234

Abstract

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.