Determination of neonicotinoid pesticides residues in agricultural samples by solid-phase extraction combined with liquid chromatography–tandem mass spectrometry

Abstract: This work reports a new sensitive multi-residue liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for detection, confirmation and quantification of six neonicotinoid pesticides (dinotefuran, thiamethoxam, clothiandin, imidacloprid, acetamiprid and thiacloprid) in agricultural samples (chestnut, shallot, ginger and tea). Activated carbon and HLB solid-phase extraction cartridges were used for cleaning up the extracts. Analysis is performed by LC–MS/MS operated in the multiple reaction monitoring (MRM) mode, acquiring two specific precursor-product ion transitions per target compound. Quantification was carried by the internal standard method with D4-labeled imidacloprid. The method showed excellent linearity (R 2 ≥0.9991) and precision (relative standard deviation, RSD≤8.6%) for all compounds. Limits of quantification (LOQs) were 0.01mgkg−1 for chestnut, shallot, ginger sample and 0.02mgkg−1 for tea sample. The average recoveries, measured at three concentrations levels (0.01mgkg−1, 0.02mgkg−1 and 0.1mgkg−1 for chestnut, shallot, ginger sample, 0.02mgkg−1, 0.04mgkg−1 and 0.2mgkg−1 for tea sample), were in the range 82.1–108.5%. The method was satisfactorily validated for the analysis of 150 agricultural samples (chestnut, shallot, ginger and tea). Imidacloprid and acetamiprid were detected at concentration levels ranging from 0.05 to 3.6mgkg−1. [Copyright &y& Elsevier]