Validation of an Analytical Method for the Determination of Pesticide Residues in Vine Leaves by GC-MS/MS

A modified and miniaturized SweEt/QuEChERS method for pesticide residue analysis applied to vine leaves is presented. The deep-frozen plant material was cryogenically processed. A 2 g analytical portion was hydrated for 30 min and extracted with acidified ethyl acetate after buffering with NaHCO3 and adding Na2SO4. A dispersive solid-phase (d-SPE) cleanup step with primary–secondary amine (PSA) was performed. The pesticide residues were determined using GC-MS/MS. The whole procedure was validated for 54–59 pesticides at 0.01, 0.02, 0.1, and 0.2 mg/kg in fresh vine leaves (Vitis vinifera). The key method performance parameters investigated were specificity, linearity, trueness, within laboratory repeatability and reproducibility, limit of detection, limit of quantitation, and matrix effects. Recoveries for the 59 pesticides tested ranged from 60 to 110%, and the RSDs were lower than 20% for the majority of the pesticides studied.