QuEChERS结合超高效液相色谱-串联质谱法同时测定畜禽肉中9种新烟碱类杀虫剂及5种代谢物残留量OA北大核心CSTPCD

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.