Determination of 15 + 1 European Priority Polycyclic Aromatic Hydrocarbons in Smoked Meat Products by Saponification/Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry.

A method for the determination of 15 + 1 European priority polycyclic aromatic hydrocarbons (EUPAHs) in smoked meat samples by saponification/solid-phase extraction and gas chromatography-mass spectrometry has been developed. Both saponification and solid-phase extraction conditions were optimized, which lead to shorter sample preparation time and excellent sensitivity and selectivity. The optimal saponification condition for the lipid extract of 5.00 g smoked food sample was 5 mL KOH (1.5 mol/L)-ethanol at 70°C for 5 min, and the shorter alkaline treatment time avoided the loss of volatile EUPAHs such as Benzo[c]fluorene. All the EUPAHs showed good linearity in the range between 5.0 and 50.0 ng/mL with correlation coefficients between 0.997 and 1.00. The estimated LODs for the EUPAHs were 0.15-0.30 μg/kg, while the LOQs were 0.50-1.0 μg/kg. The three spiking levels of EUPAHs were 1.0, 2.0 and 5.0 μg/kg, and the average recovery was between 75.2 and 99.6%, while the RSD were 2.3-12.4%. This sensitive and rapid method was successfully applied to smoked meat samples from Zhejiang Province of China, and the results revealed the presence of 13 EUPAHs. Benzo[a]pyrene (BaP) was found in 19 out of 20 samples, with concentration ranging from 0.51 to 4.57 μg/kg. The sum of concentrations of PAH4 (summation of benzo(a)pyrene, chrysene, benzo(a)anthracene, and benzo(b)fluoranthene) were 2.40-53.56 μg/kg.