The electrochemical oxidation of the antineoplastic agent etoposide was studied at carbon paste electrode in Britton–Robinson buffer solutions over the pH range 2.0—10.0 using cyclic, linear sweep and differential pulse voltammetry. Oxidation of the drug was effected in a single reversible, diffusion-controlled step within the pH range 2.0—4.0, a second oxidation process was produced above pH 4.0. Using differential pulse voltammetry (DPV), the drug yielded a well-defined voltammetric response in Britton–Robinson buffer, pH 3.0 at 0.500 V (vs. Ag/AgCl) on carbon paste electrode. This process could be used to determine etoposide concentrations in the range 2.5×10⁻⁷ to 2.5×10⁻⁵ M with a detection limit of 1.0×10⁻⁷ M. The method was successfully applied to the determination of the drug in spiked human serum.