The simultaneous determination of propranolol and pindolol using synchronous fluorescence spectrometric techniques is described. The method involves measuring the natural fluorescence of these drugs in a 50% (v/v) ethanol-water medium using zero and first derivative synchronous spectrofluorimetry. Under the optimum conditions, the linear determination ranges of propanolol and pindolol are ca. 0.02-1.0 and 0.04-1.2 mug ml(-1), respectively. The results showed that propranolol and pindolol can be determined simultaneously when the concentration ratio of propranolol to pindolol varies from 1:100 to 50:1 in the mixed sample. The method has been satisfactorily applied to the determination of propranolol and pindolol in urine samples and propranolol in pharmaceutical preparations.