Analysis of nicotinoid insecticides residues in honey by solid matrix partition clean-up and liquid chromatography-electrospray mass spectrometry

An analytical method for the routine simultaneous determination of four nicotinoid insecticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in commercial multifloral honey was developed. Fortified honey samples, dissolved in water, were cleaned up through Extrelut NT20 column and, finally, insecticides were eluted with dichloromethane. The eluate was evaporated, the residue redissolved in methanol and then analyzed by LC-ESI(+)-MS. Average recoveries of the four analytes were in the range of 76% and 99% at both spiking levels 0.1 and 1.0 mg kg−1. Relative standard deviations (RSDs) were less than 10% for all of the recovery tests. The detection limits (LODs) of the method ranged from 0.01 to 0.1 mg kg−1 for the different insecticides studied. The developed method is linear over the range assayed, 0.5-5.0 μg mL−1, with linear correlation coefficients higher than 0.9993.