Validation of a highly sensitive method for the determination of neonicotinoid insecticides residues in honeybees by liquid chromatography with electrospray tandem mass spectrometry

Abstract

The validation of a multi-residue method for the determination of five neonicotinoid insecticides (imidacloprid, clothianidin, acetamiprid, thiacloprid and thiamethoxam) in honeybees is described. The method involves the extraction of pesticides using acetonitrile and liquid partitioning with n-hexane. One clean-up is then performed on a florisil cartridge (1 g, 6 mL) and the extract is analysed by liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The recovery data were obtained by spiking honeybees samples free of pesticides at two concentration levels of the various neonicotinoids. The recoveries were in the range between 93.3 and 104.0% with relative standard deviation (RSD) less than 20%. The limit of quantification (LOQ) was 0.5 ng g−1 (corresponding to 0.05 ng bee−1) for all pesticides except for acetamiprid which was 1 ng g−1 (corresponding to 0.1 ng bee−1).