We report electrochemical preparation and characterization of poly-brilliant cresyl blue (Poly(BCB))/gold nanoparticles (Au-NPs) modified electrode. The Poly(BCB)/Au-NPs modified electrode has been used as an electrochemical sensor for the detection of hydrogen peroxide (H(2)O(2)) at lower potential (-0.2 V). The Poly (BCB)/Au-NPs film was characterized by scanning electron microscopy, Uv-visible spectroscopy (Uv-vis) and cyclic voltammetry. We have observed that, Au-NPs attached glassy carbon electrode (Au-NPs/GCE) significantly enhanced the polymerization of BCB compared to bare GCE. The Poly(BCB) film was irreversibly attached onto the Au-NPs modified electrode, the resulting hybrid film modified electrode was electrochemically active in the pH range from 2 to 11. Attachment of Poly(BCB)/Au-NPs hybrid film on the electrode surface was confirmed by Uv-vis spectra. In addition, electrocatalytic properties of the Poly (BCB)/Au-NPs/GCE towards reduction of H(2)O(2) have been investigated, and it was found that the sensitivity, reduction potential as well as the corresponding detection limit were improved as compared to the voltammetric response of the Poly(BCB)/GCE and Au-NPs/GCE. Based on this study, a non-enzymatic electrochemical sensor for the determination of H(2)O(2) has been reported. Moreover, analysis of commercial H(2)O(2) samples was performed using the proposed method and satisfactory results were obtained. (C) 2010 Elsevier B.V. All rights reserved.