The HPLC method for the determination of sotalol (SOT), metoprolol (MET) and alpha-hydroxymetoprolol metabolite (MET-H), paracetamol (PAR), paracetamol glucuronide (PAR-G) and paracetamol sulfate (PAR-S) in human urine is described. Analyses were carried out on a reversed-phase LiChroCART Purospher C18e column (125 mm x 3 mm, 5 microm particles) (Merck) with gradient elution as well as spectrophotometric and fluorometric detection. Good resolution of the analyzed substances was obtained within a time range of no longer than 15 min. The linearity ranges of the callibration curves in human urine (as matrix) were: 3.25-45 microg ml(-1) (SOT), 0.75-40 microg ml(-1) (MET), 0.6-40 microg ml(-1) (MET-H), 4.6-60 microg ml(-1) (PAR-G), 4.95-50 microg ml(-1) (PAR-S), 1.95-45 microg ml(-1) (PAR). An application to human urine samples was performed.