A simple and sensitive method for the quantitative determination of salbutamol in human serum using reversed-phase ion-pair high-performance liquid chromatography with electrochemical detection is described. The method involves the combined use of Sep-Pak cartridges and ion-pair extraction for sample clean-up, and subsequent separation of salbutamol and the internal standard from interfering compounds on a reversed-phase column. An amperometric detector incorporating a glassy carbon electrode was employed for detection. The inter-assay coefficients of variation at plasma concentrations of 2.0, 6.0 and 20.0 ng/ml were 7.3%, 7.2% and 8.5%, respectively (n = 20). The minimum detection limit was 400 pg/ml from a 0.5-ml sample of serum. The method can be readily utilised for clinical pharmacokinetic studies.