Isotope-labeled internal standards and grouping scheme for determination of neonicotinoid insecticides and their metabolites in fruits, vegetables and cereals – A compensation of matrix effects

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Neonicotinoid insecticides (NIs) are widely used. However they produce high levels of residues and are toxic to non-target organisms, especially when their metabolites exhibit comparable or elevated toxicities. In this study, we established a multi-residue analytical method for analyzing 20 compounds – 8 NIs and their 11 major toxic metabolites. QuEChERS pretreatment and ultra-high-performance liquid chromatography–tandem mass spectrometry were used to detect residues in fruits, vegetables and cereals. Determination time was shortened to 6 min. Average recoveries of all compounds were in the range of 90.1–105.5%, with relative standard deviations lower than 15.0% and the limit of quantitation being 10 µg kg−1. For the first time, 8 NIs and 11 major toxic metabolites were grouped simultaneously, such that the matrix effect of analytes was satisfactorily corrected using their own isotopically labeled molecules; other NIs and metabolites in the same group were also corrected. This is the first report that simultaneously quantified multiple metabolites of eight NIs in multiple matrices.