Abstract:Objective To establish an analysis method for the simultaneous determination of 10 neonicotinoid pesticide residues in raw milk by dispersive solid-phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS).Methods The samples are extracted with acetonitrile, salted out with a QuECHER salt pocket, and purified by the dispersive solid-phase extraction (d-SPE) method. The analytes are detected by UPLC-MS/MS and quantified by the external standard method.Results 10 targeted compounds show a good linear relationship in a certain concentration range with the coefficient of determination (R2) over 0.999. The limits of detection (LODs) are 0.2~0.5 μg/kg, while the limits of quantification (LOQs) are 1.0 μg/kg. At the supplemental levels of 1.0, 2.5, and 5.0 μg/kg, the average recovery rates of standard addition of analytes in raw milk are between 75.9%~108.9%, with the intra-day precision (RSDr) of 1.8%~7.6% and the inter-day precision (RSDR) less than 11.7%.Conclusion The established method is simple for pretreatment and has good repeatability and high sensitivity. It is suitable for the detection of neonicotinoid pesticide residues in raw milk.