Copper oxide impregnated gamma-Al2O3 hybrid catalysts (5 to 25 wt%CuO@Al2O3) were prepared and characterized by XRD, FT-IR, SEM, and EDX. The redox properties of the materials were studied electrochemically which coincided well with the XRD and EDX analyses. Their catalytic properties were comprehended using electrochemical impedance, cyclic voltammetry, and chronoamperometry. All samples showed potentiality for electrocatalysis; 20CuO@Al2O3 was found to exhibit highest accessible surface area, lowest charge transfer resistance and hence better potentiality as electrocatalyst. This composition mediated a fast electron transfer for electroxidation of both the methanol and glucose. The material possessed appreciable sensitivity of 35.6 mu A mM(-1) cm(-2) with a wide detection range (2-20 mM) for glucose oxidation. The electrode demonstrated reproducibility, stability, and sensitivity via application study of two analytes. The prominent outcome of the present study was optimal loading of CuO onto gamma-Al2O3 for electrocatalysis. (C) 2015 The Electrochemical Society. All rights reserved.