Comparing d-SPE Sorbents of the QuEChERS Extraction Method and EMR-Lipid for the Determination of Polycyclic Aromatic Hydrocarbons (PAH4) in Food of Animal and Plant Origin

A Quick, Easy, Cheap, Rugged, Effective, and Safe (QuEChERS) method for the determination of benzoa]anthracene, chrysene, benzob]fluoranthene, benzoa]pyrene (PAH4 including the interfering PAHs triphenylene, cyclopentac,d]pyrene, benzok]fluoranthene, benzoj]fluoranthene) was developed and validated with GC-MS/MS in foods of plant and animal origin. PAHs were extracted with acetonitrile, and different clean-ups with various compositions of sorbents, including zirconia-based sorbent (Z-Sep), primary-secondary amine (PSA), anhydrous magnesium sulfate (MgSO₄), octadecylsilane (C18 endcapped), and enhanced matrix removal (EMR)-lipid material, were tested. Another important focus of this study was the separation of critical pairs, which is essential for the qualification and quantification of PAH4. To investigate the developed methods, samples were spiked beneath their maximum levels (MLs) and recoveries and peak shapes were compared. The clean-up with 900 mg MgSO₄ + 150 mg PSA + 150 mg C18 was chosen to be validated in salmon, mussels, shrimps, bacon, cutlets, wheat flour, curry spice powder, infant formula, infant follow-up formula, and infant foods. Recoveries for all analytes were between 75 and 108%, combined with standard deviation between 2 and 20%. Limits of detection (LODs) and limits of quantification (LOQs) were between 0.04 and 0.34 μg/kg and between 0.1 and 1 μg/kg, respectively.