The volatile amines dimethylamine (DMA) and trimethylamine (TMA) are common degradation products of TMA-oxide in marine fish. Both compounds are used as important indicators of quality in seafoods. DMA is produced along with an equimolar quantity of formaldehyde by action of an endogenous enzyme found primarily in gadoid fish. TMA is produced in fresh, but not frozen seafoods by a bacterial enzyme. The current AOAC method for determination of TMA in fish is based on the colorimetric estimation of TMA as a picrate salt. This method is not specific for TMA; ammonia, monomethylamine, and DMA also form corresponding picrate salts. Gas chromatography provides a means of separating and quantitating the individual volatile amines. A simple perchloric acid extract of fish is neutralized with potassium hydroxide and extracted with benzene. The amines are then separated by gas chromatography on a porous polymer packed column and detected by using a nitrogen-phosphorus-specific flame ionization detector. The method provides simple, rapid simultaneous quantitation of DMA and TMA, and is applicable to a wide variety of seafoods.