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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.