The redox equilibriums involving zearalenone were studied by cyclic and differential pulse voltammetry on a glassy carbon electrode. The cyclic voltammograms of zearalenone in DMSO at a glassy carbon electrode in the potential range from −600 to 1400 mV vs. the Ag/AgCl have two oxidation peaks and a reduction one. Zaralenone concentration may be determined by DPV at +1050 mV. The method was applied to the determination of zearalenone concentration in corn, barley, and maize. Studies performed in aqueous solution or in mixed solvents water-acetonitrile containing 1 M H2SO4 showed that the oxidation of ZEN with an aqueous solution of Ce(IV) at room temperature, in the dark, occurs with the destruction of ZEN molecule. Studies performed in aqueous solution or in mixed solvents water-acetonitrile containing 1 M H2SO4 showed that the oxidation of ZEN with an aqueous solution of Ce(IV) at room temperature, in the dark, occurs with the destruction of ZEN molecule.