A new, simple and selective differential pulse voltammetry (DPV) method for the simultaneous determination of selected drugs in model solutions and spiked human urine samples with prior extraction was developed and validated. The objects of analysis were paracetamol, furosemide, dipyrone, cefazolin and dexamethasone belonging to four different therapeutic groups (antibiotics, analgesic, demulcent and diuretic). Analytical methods for the preparation of urine samples for voltammetric analysis (liquid-liquid extraction--LLE and solid-phase extraction--SPE) were worked out and optimized. Hanging mercury drop electrode (HMDE) and graphite electrode were used as working electrodes. Reference electrode was Ag|AgCl|KCl((sat.)), whereas auxiliary electrode--platinum electrode. The optimal conditions for quantitative determination were obtained in a Britton-Robinson (BR) buffer at pH 2.4. Quantification was performed by means of calibration curve and standard addition methods. The calibration curves of analysed drugs are linear within the range of concentration: 6.61-66.10, 6.05-54.42, 6.00-65.00, 4.20-33.58 and 0.51-3.06 microM for paracetamol, furosemide, dipyrone, cefazolin and dexamethasone, respectively. The levels of analysed compounds in human urine can be successfully determined using this developed method with no matrix effect.