Liquid chromatography-tandem mass spectrometric methods for the determination of spinosad, thiacloprid and pyridalyl in spring onions and estimation of their pre-harvest interval values

Two liquid chromatography-tandem mass spectrometric methods were developed and validated to determine spinosyn A and D, thiacloprid and pyridalyl in spring onions cultivated under Egyptian field conditions. The degradation rates, the pre-harvest interval (PHI) values and the half-life values of the three pesticides were estimated. QuEChERS was used for sample preparation and the separation was performed on an X-Bridge C18 column with ACN-formic acid 0.1% as the mobile phase. Linear range, method detection limits (MDLs), precision, recovery and matrix effects were estimated. The multi-residue MDLs ranged from 0.02 μg/kg (spinosyn A & D) to 0.05 μg/kg for pyridalyl. All the investigated pesticides showed high degradation rates. For spinosad the half-life value was 1.2 days, for thiacloprid it reached 2.2 days and for pyridalyl 4.4 days. Furthermore, the calculated PHI values, according to the maximum residue levels set by the EU, were 0 days for spinosad, 9.8 days for thiacloprid and 39.4 days for pyridalyl.