The antibacterial drug, nitrofurazone [5-nitro-2furaldehyde semicarbazone] a synthetic nitrofuran derivative, was reported to possess good bacteriostatic and bactericidal properties, has an antibacterial action against a number of Gram-negative and Gram-positive micro-organisms [1,2] and is used for the treatment of burns [3] and trypanosomiasis [4]. In veterinary medicine nitrofurazone is used for the treatment and prophylaxis of coccidiosis in poultry and farm animals, and necrotic enteritis in pigs [1]. The determination of some nitrated heterocyclic compounds containing reduction sites similar to that of nitrofurazone was studied by Vignoli et al. [5] using Brittion–Robinson (BR) buffer pH of between 1.81 and 11.98. Various methods including spectrophotometry [6,7], turbidity [8], colorimetry [9,10], conductimetry [11], paper chromatography [12] and high performance liquid chromatography [13,14] have determined nitrofurazone in its pharmaceutical preparations. A little attention has been paid to the polarographic determination of nitrofurazone [15–18] or to the electrochemical behaviour of this compound [19,20]. A rotating platinum electrode was used to study nitrofurazone by a simple direct current procedure [21–24]. The present work is a continuation of our studies in the field of the determination of the antibacterial drugs using cathodic stripping voltammetry (CSV) at the hanging mercury drop electrode (HMDE) [25]. This technique offers a high senstivity with respect to the other analytical techniques [26]. The aims of this study are to establish the experimental conditions, to investigate the adsorptive voltammetric behaviour of nitrofurazone and to optimize the conditions for determination of the titled compound in pharmaceutical formulations present in urine and serum. * Corresponding author.