The electrooxidation of mitoxantrone (MXT) on carbon paste electrodes was studied using voltammetric techniques in adsorption conditions. The analyte was accumulated at the working electrode (a carbon paste electrode) under precisely controlled mass-transport conditions and stripped electrochemically in the same solution. An electrode pretreatment is proposed which shows good reproducibility of the analytical signal (0.81%). The stripping step was studied with alternating current voltammetry providing a linear response in the concentration range 5 x 10(-11) to 7 x 10(-10)M in aqueous samples. Finally, a method using the medium exchange and AC phase-selective adsorptive stripping voltammetry technique was proposed for MXT analysis in urine samples.