Amethod is described for the sample clean‐up and estimation of nitropolycyclic aromatic hydrocarbons (nitro‐PAH) in foods. The analysis involves the novel use of a coupled capillary gas chromatograph/thermal energy analyser and provides a detection limit for 1‐nitropyrene of 12 pg (equivalent to 0·02 μg/kg for a 50‐g sample). Only 3 out of 24 samples contained detectable quantities of nitro‐PAHs; these were in the range 0·2–2·0 μg/kg. In contrast to the widespread occurrence of the parent PAHs in foodstuffs, the presence of nitro‐derivatives appears to be minimal.