Simultaneous Determination of Nine Neonicotinoid Insecticides and Five Metabolites in Meat by QuEChERS Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

In this study, a method for the simultaneous determination of neonicotinoid insecticides and their metabolites in meat was established by the QuEChERS (quick, easy, cheap, effective, rugged, safe) pretreatment method followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with acetonitrile containing 1% acetic acid. After salting-out with 1 g of NaCl and 4 g of anhydrous MgSO₄, the supernatant was cleaned-up using C₁₈. The separation of the analytes was carried out on a XSelect HSS T3 (150 mm × 3.0 mm, 2.5 μm) column by gradient elution with a mobile phase composed of 0.1% formic acid and acetonitrile. The analytes were detected by multiple reaction monitoring (MRM) in the positive ion mode and quantified by the matrix-matched external standard method. The results showed that the calibration curves for all analytes had a good linearity with correlation coefficients (r) more than 0.995. The limit of quantitation (LOQ) was 2 μg/kg for 12 target compounds and 20 μg/kg for the two compounds. The recovery rates of the proposed method were in the range of 61.0%–116.7% with relative standard deviations (RSDs) below 14.81%. This method has the merits of simple pretreatment steps and satisfying recovery rates and enables fast and accurate detection of neonicotinoid insecticides and their metabolites in meat.