A technique for the analysis of the volatile compounds from fish tissue employing microwave distillation-solid-phase microextraction-gas chromatography-mass spectrometry is described. A qualitative listing of 174 compounds observed in the headspace is given, and a quantitative method for the determination of the off-flavor contaminants (2-methylisoborneol and geosmin) is presented. Borneol and decahydro-1-naphthol are used as the surrogate and internal standards, respectively. A linear calibration curve is obtained for 0.1 to 5 ppb with a recovery level of 60% at 2.5 ppb. Comparison of the instrumental method with a human flavor checker showed good agreement.