Determination of neonicotinoids and 199 other pesticide residues in honey by liquid and gas chromatography coupled with tandem mass spectrometry

Abstract

Current work presents a modified QuEChERS method for the determination of 207 pesticide residues in honey by LC-MS/MS and GC-MS/MS. Acetate buffered acetonitrile extraction with Z-Sep+ and PSA dispersive-SPE clean-up were used for sample preparation. Optimised conditions allows determination of neonicotinoids as well as other insecticides, fungicides, herbicides, acaricides, growth regulators and veterinary drugs in honey samples. Validated method enable sensitive analysis at least at concentrations from 0.001, 0.005 or 0.01 mg/kg for 45%, 41% and 14% of pesticides, respectively. Method was utilised for the analysis of 155 honey samples from Poland during 2015-2017. Residues of 21 pesticides were determined in honey. Cyano-substituted neonicotinoids (acetamiprid, thiacloprid) were quantified in 77% of samples and were the most frequently detected pesticides. Concentrations of acetamiprid was from 0.001 to 0.13 mg/kg whilst thiacloprid from 0.001 to 0.2 mg/kg. Fungicides were determined in 50% and amitraz metabolites in 35% of honey samples.

Keywords: GC–MS/MS; Honey; LC–MS/MS; Neonicotinoids; Pesticide residues; QuEChERS; Triazoles.