The study uses gas chromatography with tandem mass spectrometry (GC-MS/MS) to develop a reliable analytical approach for detecting multiclass pesticides, polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) in poultry meat and chicken eggs. The meat (2 g) and egg (4 g) samples were extracted with acidified acetonitrile (10 mL) as part of the optimized sample preparation technique. The cleanup consisted of freezing an aliquot of the extract (5 mL) at −20 °C, followed by dispersive solid phase extraction using 50 mg PSA + 100 mg C18+150 mg MgSO4. The matrix co-extractives were effectively removed and the method performance met the European Commission’s analytical quality control criteria (SANTE/12682/2019). The method was validated at two spiking levels (10 and 20 ng/g of 225 pesticides, 9 PAHs and 8 PCBs), and good recoveries (70–120%) and precision-RSDs (≤20%) were achieved for 90% of the targeted pesticide residues. For 80% of the compounds, the LOQs were ≤10 ng/g. The results of the intra-laboratory (involving six analysts) and inter-laboratory validation studies (involving eight ISO 17025 accredited laboratories) established satisfactory ruggedness and reproducibility. It created potential applications in commercial residue testing laboratories for regulatory compliance check purposes.
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