A new method for the qualitative and quantitative determination of trenbolone and testosterone residues in meat, liver, and kidney is described. The analytical procedure consists of the following steps: homogenisation of the meat sample with tetrahydrofurane; liquid-liquid partition first between acetonitrile and hexane, then between sodium hydroxide and petroleum ether/benzene; purification of a silica gel column. The purified sample is analysed by high pressure liquid chromatography using silica gel packings. Detection and quantitative determination are performed with a fluorescence and/or a spectrophotometric detector. Fluorescence measurements are carried out applying a self-made silica gel packed flow-cell. The detection limit in meat extracts is 50 ppb for testosterone and 5 ppb for trenbolone.