The electrochemical reduction behavior o f nicournalone has been studied by using dc polarography, cyclic voltammetry, ac polarography, differential pulse polarography, millicoulometry, and controlled potential electrolysis in universal buffers ranging from pH 2.0 to 12.0 in DMF-water mixtures. Kinetic parameters such as diffusion coefficient ( D ) and forward rate constant (k;J values are evaluated and a reduction mechanism is proposed. A simple and rapid differential pulse polarographic method has been developed for the determination of nicoundone in pharmaceutical formulations using the standard addition method. The detection h i i t is 2.7 ng mL-'.