The electrochemical behaviour of xipamide was studied at glassy carbon electrode in Britton-Robinson buffer solution of different pH values ranging from 2.0 to 7.0 using cyclic voltammetry and square wave voltammetry. Voltammetric results showed a reversible redox and diffusion-controlled process. The oxidation and reduction peaks were found at potentials of 0.375 V and 0.321 V at pH 5.0, respectively. While the reported voltammetric method 2 shows irreversible oxidation process for xipamide and having higher detection limit than the proposed method. Linear responses were obtained over concentration ranges of 5.0 × 10-8 to 6.46 × 10-7 mol L-1 and 5.0 × 10-8 to 9.90 × 10-7 mol L-1 with detection limits of 3.97 × 10-9 mol L-1 and 3.30 × 10-9 mol L-1 for oxidation and reduction processes, respectively. Sensitivity, precision and accuracy were evaluated. The proposed method is suitable for the quality control of xipamide in bulk, commercial formulations and urine.