Fluvalinate residues in honey by capillary gas chromatography—Electron capture detection—Mass spectrometry

A fast, simple and accurate analytical method for determination of residual Fluvalinate in honey is described. Honey sample was dissolved in methanol-water and Fluvalinate extracted with ethyl acetate. The organic phase was evaporated and the residue dissolved in ethyl acetate. After clean-up on a C18 Sep-Pak cartridge Fluvalinate was eluted withn-hexane, concentrated under a stream of nitrogen and analysed by capillary GC-ECD-MS in selected-ion monitoring mode. Recoveries from honey samples spiked at 7 fortification levels (0.01–50 ng g−1) range from 93.8–100.2%, RSD≤5.0%. The limit of detection was 8 ng g−1 in GC-ECD and 18 ng g−1 in GC-MS (SIM) with RSDs of 7.2 and 6.8% respectively. The method was used to analyse several types of honey (60 samples) from different Italian regions. Fluvalinate residues were detected in these samples and concentrations ranged from LOD to 0.09 ng g−1.