A fit-for-purpose method to monitor 16 European Union PAHs in food: results of five years of official food control in two Italian regions

Abstract

ABSTRACTA gas-chromatographic single-quadrupole analytical method for the analysis of the 16 priority European Union (EU) polycyclic aromatic hydrocarbons (PAHs) in food is presented. The method fulfils the request of Regulation EU 836/2011 for an analytical procedure to be used for official control of PAHs in food in EU member states. The sample preparation involves a pressurised liquid extraction (PLE) with an in-cell clean-up step followed by a lipid removal using solid-phase extraction (SPE) on a styrene divinylbenzene stationary phase (SDVB) and a final gel-permeation chromatography (GPC) step. To reach a better sensitivity for all the analytes, including the heaviest last eluting PAHs, 3 μl of the purified extract were injected in solvent vent mode using a programmable temperature vaporization (PTV) injector. The isobaric PAH isomers were successfully separated using an Agilent Technologies DB-17MS (20 m × 0.18 mm × 0.18 μm) column. The method was fully validated using an in-house approach and the sensitivity, accuracy and precision obtained were satisfactory. The method expanded uncertainty was estimated and it was verified that it was below the maximum standard measurement uncertainty. Moreover, the results of 347 samples of meat and meat products, fish and fish products and mussels collected from January 2012 to December 2016 in the Marche and Umbria regions of Italy are reported. None of the samples exceed the maximum levels fixed by EU Regulation 835/2011, and clams turned out to be the most contaminated among the food matrices analysed. Finally, an estimate of the sum of four marker PAHs (benzo[a]anthracene, benzo[b]fluoranthene, benzo[a]pyrene, chrysene) as indicator of the PAHs contamination was done by comparison with the 16 carcinogenic PAHs sum.