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

Abstract

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 5.00g smoked food sample was 5mL KOH (1.5mol/L)-ethanol at 70°C for 5min, 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 50.0ng/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.