A method for the determination of toxaphene residues in fish and fish-based baby foods has been developed. The cleanup of the fatty matrices was performed using an acid treatment on an Extrelut-NT3 and ENVI-Florisil SPE cartridges system, using light petroleum as eluent. Instrumental analysis was carried out by gaschromatography with mass spectrometry detector (GC/MS) in SIM mode. Recoveries from spiked samples were tested at 0.005 and 0.01 mg/kg per single congener and were in the range 82-104% while relative standard deviations (RSDs) were in the range 3.7-10.9%. Nineteen samples of both frozen fish food and fish-based baby foods representative of the Italian market were collected from local dealers and analysed.