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Validation of QuEChERS for screening of 4 marker polycyclic aromatic hydrocarbons in fish and malt.

Duedahl-Olesen, L., Iversen, N.M., Kelmo, C., Jensen, L.K.
Food control 2018
European Union, anthracenes, barley, benzo(a)pyrene, cold, mackerel, malt, peat, screening, smoked salmon, zirconium
Application of QuEChERS as a new quick and easy method for screening of polycyclic aromatic hydrocarbons (PAHs) was developed, validated and used for quantification (GC-QTOF-MS) of 4 PAHs, namely benz[a]anthracene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene. A clean-up step using Zirconium based dispersive SPE was applied. Validation based on spiked samples (0.5, 1 and 4 μg/kg) revealed a limit of quantification (LOQ) for the 4 PAH compounds in the range of 0.14–0.24 μg/kg for fish and 0.12–0.24 μg/kg for raw barley. Overall recoveries ranged from 88 to 117% with repeatability and in-house reproducibility from 2.6 to 16%. The method was applied to 9 malt samples which were found to contain the sum of 4 PAH from <0.36 μg/kg for raw barley to 26 μg/kg for peat smoked barley. For 5 smoked fish samples the sum of PAH4 ranged from <0.34 μg/kg for cold smoked salmon to 2.2 μg/kg for hot smoked mackerel. In general it was found that the method could be used as a fast screening for evaluation of smoked fish according to EU Commission maximum concentrations of benzo[a]pyrene (2.0 μg/kg) and the sum of PAH4 (10 μg/kg).