Determination of acetamiprid, imidacloprid, and spirotetramat and their relevant metabolites in pistachio using modified QuEChERS combined with liquid chromatography-tandem mass spectrometry

A QuEChERS based methodology was developed for the simultaneous identification and quantification of acetamiprid, imidacloprid, and spirotetramat and their relevant metabolites in pistachio by liquid chromatography-tandem mass spectrometry for the first time. First, sample extraction was done with MeCN:citrate buffer:NaHCO3 followed by phase separation with the addition of MgSO4:NaCl. The supernatant was then cleaned by a primary-secondary amine (PSA), GCB, and MgSO4. The proposed method provides a linearity in the range of 5-200 µg L−1, and the linear regression coefficients were higher than 0.99. LOD and LOQ were obtained to be 2 and 5 µg kg−1 for the studied insecticides, respectively, with the exception of imidacloprid-olefin (5 and 10 µg kg−1). Acceptable recoveries (91-110%) were obtained for all the analytes with good intra- and inter-precisions (0.4 ≥ RSD ≤11.0). The method was then used for the pistachio samples collected from a field trial to estimate the maximum residue limits (MRLs) in next step.