A sensitive adsorptive stripping voltammetric method for the measurement of cilazapril in 0.04 M Britton-Robinson buffer (pH 9.0) solution was described. The method was based on the adsorptive accumulation of the drug at a hanging mercury drop electrode (HMDE), followed by differential pulse voltammetry. The response was evaluated with respect to pre-concentration time, pH effect, accumulation potential, accumulation time and scan rate. The peak potential was -0.60 V (vs. Ag/AgCl). The peak current was directly proportional to the concentration of cilazapril with a detection limit of 17.6 ng ml(-1) at an accumulation time of 10 s. The reduction process was irreversible and the wave showed adsorptive characteristics. The results were compared to those obtained using a HPLC procedure. A reversed-phase C18e column with aqueous phosphate buffer (pH 3.5; 0.125 M)-acetonitrile (67:33, v/v) mobile phase and benazapril as internal standard was used. UV detector was set at 254 nm. Results obtained in HPLC were comparable to those obtained by adsorptive stripping voltammetric method. (C) 2002 Elsevier Science B.V. All rights reserved.