Two different approaches to the analysis of nitrated polycyclic aromatic hydrocarbons (nitro‐PAHs) in food samples are presented, based on liquid chromatography with fluorescence detection and gas chromatography with a mass selective detector as the alternative method. For the HPLC analysis the nitro‐PAHs at trace level concentrations are efficiently reduced to primary aromatic amines on a catalyst column packed with 5 μm alumina coated with platinum and rhodium. The particulate extraction/fractionation procedure is discussed and the results of both methods are compared. The concentrations of seven nitro‐PAHs in grilled and smoked food are presented.