A method has been developed for the simultaneous determination of the sympathomimetic drugs salbutamol and terbutaline in the plasma of poisoned patients, using ion-pair high-performance liquid chromatography with amperometric detection. Plasma concentrations of the drugs, measured in 8 poisoned patients, were well above the therapeutic range. The clinical and metabolic effects of overdose with these drugs were considerably less severe than those seen in patients with plasma theophylline concentrations elevated to the same degree.