Hollow CuO/Fe2O3 hybrid microspheres with small uniform holes were synthesized using a convenient hydrothermal method and were applied to fabricated an amperometric sensor for kojic acid. The resulting materials were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) and then were immobilized into the chitosan (Chi) matrix onto a glassy carbon electrode to obtain CuO/Fe2O3-Chi/GCE. The potential utility of the constructed electrodes were demonstrated by applying them to the analytical determination of kojic acid concentration. The electrochemical behavior of kojic acid on CuO/Fe2O3-Chi/GCE was explored. The modified electrode displayed excellent amperometric response for kojic acid with a linear range from 0.2 mu M to 674 mu M with a detection limit of 0.08 mu M at a signal-to-noise ratio of 3. In order to validate feasibility, the CuO/Fe2O3-Chi/GCE has been used for quantitative detecting kojic acid in real samples. (C) 2010 Elsevier Ltd. All rights reserved.