A method has been developed for the determination of clenbuterol in bovine urine using differential-pulse voltammetry (DPV), based on the electrochemical behaviour of clenbuterol at a Nafion-modified carbon paste electrode (CPE). Clenbuterol is irreversibly oxidized at high positive potentials, its irreversibility being due to a chemical follow-up reaction which results in a product showing quasi-reversible electrochemical behaviour at much lower potentials. It is the oxidation peak of this product, arising in acidic media at 0.42 V, which was analysed using DPV, again following the accumulation of clenbuterol at the Nafion-modified CPE. Electrode renewal was achieved by holding the potential at -0.6 V for 120 s in 0.1 mol l-1 NaOH. The determination of clenbuterol in the presence of interfering compounds present in bovine urine samples was then carried out after a two-step clean-up of the urine involving liquid-liquid extraction followed by a mixed-mode solid-phase extraction procedure. This allowed clenbuterol to be detected down to a level of 1.02 x 10(-9) mol l-1 in bovine urine extracts.