Clenbuterol, a beta-agonist, was determined in samples of beef liver and muscle. The method employed an acidic aqueous extraction followed by protein precipitation. The supernatant liquid was passed through a weak cation-exchange cartridge and then through a commercially available immunoaffinity cartridge. Clenbuterol was eluted from the immunoaffinity cartridge with 80% ethanol in water. The eluate was concentrated and analysed directly by reversed-phase liquid chromatography using gradient elution and UV detection at 245 nm. Detection limits were estimated to be 0.3 ng g −1 clenbuterol. A single immunoaffinity cartridge was used for ten sample extracts with no significant loss in capacity. No organic solvents other than ethanol and methanol were employed in the procedure. Recoveries of clenbuterol from samples of beef liver and muscle spiked at 2 and 5 ng g −1 carried through the entire procedure were 63±11% (range, 53–74%) compared to pure standards. Absolute recoveries of pure standards (30 ng clenbuterol) carried through the same analytical steps were 70±5% ( n = 6), the losses being primarily due to the ion-exchange step.