A procedure for the simultaneous quantitative determination and selective identification of potassium canrenoate and butizide is proposed. The amount of canrenone, the degradation product of potassium canrenoate, is also determined. Elution of these compounds is investigated on LiChrosorb RP-18 and RP-8 columns. The analysis time was shorter on a RP-8 column while the specific identification was still possible. Therefore, the LiChrosorb RP-8 column was chosen. The eluent consisted of an acetonitrile--0.05 M phosphate buffer, pH 4 (45:55) mixture. Quantitative determination was performed at the absorption maximum of each compound: 286 nm for potassium canrenoate and for canrenone, 271 nm for butizide. This change in wavelength is performed automatically by the computer that controls the spectrophotometric diode array detector.