The March 1989 oil spill in Alaska prompted the Food and Drug Administration (FDA) to conduct a thorough investigation of clean‐up methodologies aimed at determining low ng/g (ppb) levels of polynuclear aromatic hydrocarbons (PAHs) in seafood. The clean‐ups from a modified FDA method and a National Marine Fisheries Service (NMFS) method were evaluated on the basis of the determination of 18 PAHs at levels ranging from 1 to 5 ppb by gas chromatography/mass spectrometry. In the modified FDA method, seafood extracts were purified by a liquid‐liquid partition followed by a three‐step elution through silica, alumina, and C18solid‐phase extraction cartridges. In the NMFS method, seafood extracts were purified by column chromatography through a deactivated silica gel/alumina column and a gel permeation high performance liquid chromatography column. Both methods quantitated 18 PAHs at levels ranging from 1 to 5 ppb. With the exception of naphthalene, average recoveries based on internal deuterated standards ranged from 73 to 144% for the modified FDA method and 63 to 106% for the NMFS method.