A sample preparation methodology using different d-spe sorbent for amitraz analysis in honey

Abstract

An analytical method was validated using gas chromatography with tandem mass spectrometry (GC/MS) for the precise analysis of amitraz and its metabolites 2, 4- dimethylaniline (2, 4 - DMA) in honey. The QuEChERS technique, which comes from the words Quick, Easy, Cheap, Effective, Rugged, and Safe extraction of the pesticides was used. Amitraz is both an acaricide and insecticide and is often used in beekeeping to protect honeybee colonies against Varroa destructor. The procedure was validated according to SANTE/11325/2021 and the values of recovery, precision, and linearity, limit of detection and limit of quantification were established. The average recoveries obtained for amitraz were ranged from 79.4 to 100.8% and for 2, 4 dimethylaniline from 78.1% to 103.6 % at the two spiked levels 0.01 and 0.02 mg/kg. Several clean-up approaches were tested: d-SPE with Enhanced Matrix Removal-Lipid (EMR-Lipid), combination of anhydrous magnesium sulfate, primary secondary amine (PSA) and C18 sorbents, and a third method using Z-Sep. The most precise recovery, i.e. the highest accuracy, was achieved using purification with EMR lipid. The linearity of the analytical response across the studied range of concentrations (0.010 - 0.10 mg/kg) was excellent, obtaining correlation coefficients higher than 0.99. Limit of quantification was 0.004 mg/kg for amitraz and 0.005 mg/kg for 2, 4-DMA. The method was used for the determination of amitraz and 2, 4-DMA in real samples of acacia and flower honey.