Development and validation of an analytical method for the multiresidue analysis of pesticides in sesame seeds using liquid- and gas chromatography with tandem mass spectrometry

For the first time, an analytical method for the multiresidue analysis of multiclass pesticides in sesame seeds using liquid- and gas chromatography with tandem mass spectrometry (LC-MS/MS and GC-MS/MS) was developed and validated. At first, the sample was comminuted after adding water (1:2 w/v). The sample preparation workflow included acetonitrile extraction, followed by freeze-out of the extract at -80°C with a subsequent cleanup by dispersive solid phase extraction (dSPE) (100 mg of C₁₈ + 150 mg of MgSO₄ for LC-MS/MS and 100 mg of C₁₈ + 25 mg florisil + 150 mg of MgSO₄ for GC-MS/MS). As noted, these cleanup steps were quite effective in removing the fatty co-extractives. The optimised sample preparation method effectively minimised the matrix effects and offered a limit of quantification (LOQ) of 0.01 mg/kg for most compounds. The LC-MS/MS and GC-MS/MS methods were validated at three levels (0.01, 0.02 and 0.05 mg/kg) for 222 and 220 compounds respectively. The method accuracy and precision complied with the performance criteria of the SANTE/12682/2019 analytical quality control procedure. The results of the intra-laboratory (involving six analysts) and inter-laboratory studies (involving eight accredited laboratories) were comparable for all pesticides. Considering its performance efficiency and alignment with the regulatory guidelines, this method can be implemented across the food testing laboratories for the monitoring of pesticide residues in sesame seeds.