A high-performance liquid chromatographic (HPLC) method for sotalol in biological fluids is presented. Sample preparation involves a simple acid-base double-extraction procedure, and analysis is carried out on a reversed-phase chromatographic system using a muBondapak C18 column. Procainamide was used as the internal standard. As little as 20 ng of sotalol/ml can be detected with good precision by a fluorometric detector. HPLC, which allows more rapid analysis of plasma sotalol levels than does GLC, appears suitable for pharmacokinetic studies as well as for therapeutic drug monitoring.