A fit-for-purpose method to monitor 16-EU-PAHs in food - results of five year official food control in two Italian regions

A gas-chromatographic single quadrupole analytical method for the analysis of the sixteen priority EU 6 Polycyclic Aromatic Hydrocarbons (PAHs) in food is here presented. The method fulfils the request of 7 Regulation EU 836/2011 for analytical procedure to be used in official control of PAHs in food, in European 8 Union member states. The sample preparation involves a Pressurised Liquid Extraction (PLE) with an in cell 9 clean-up step followed by a lipid removal SPE on a styrene divinylbenzene stationary phase (SDVB) and a 10 final Gel Permeation Chromatography (GPC). To reach a better sensitivity for all the analytes, included the 11 heaviest last eluting PAHs, three microliter of the purified extract were injected in Solvent Vent Mode using 12 a Programmable Temperature Vaporization (PTV) injector. The isobaric PAH isomers were successfully 13 separated using anAgilent Technologies DB-17MS (20m × 0.18mm x 0.18μm) column. The method was 14 fully validated using an in house approach and the sensitivity, accuracy and precision obtained were 15 satisfactory. The method Expanded Uncertainty was estimated and it was verified that it was below the 16 maximum standard measurement uncertainty. Moreover, the results of three hundred and forty seven samples 17 of meat and meat products, fish and fish products and mussels collected from January 2012 until December 18 2016 are reported. None of the samples exceed the maximum levels fixed by EU Regulation 835/2011 and 19 clams turned out to be the most contaminated among the food matrices analysed. Finally an estimate of the 4 20 markers sum (Benzo[a]anthracene, Benzo[b]fluoranthene, Benzo[a]pyrene, Chrysene) as indicator of the 21 PAHs contamination was done by comparison with the 16 carcinogenic PAHs sum.