Hydroxypropyl-beta p-cyclodextrin-reduced graphene oxide hybrid nanosheets (HP-beta-CD-RGO) were synthesized by microwave irradiation and characterized by transmission electron microscopy, atomic force microscopy and thermal gravimetric analysis. The hybrid nanosheets, combining Nafion and in situ deposited bismuth film, were used as the sensing material for the simultaneous determination of Pb2+ and Cd2+ for the first time. Cyclic voltammetry and electrochemical impedance spectroscopy were used to investigate the electrochemical properties of HP-beta-CD-RGO, and the results suggested that this hybrid nanosheets possessed good electrochemical catalytic activity. Compared with HP-beta-CD and graphene, the stronger square anodic stripping voltammetric responses for Pb2+ and Cd2+ were observed on HP-beta-CD-RGO modified glassy carbon electrode, which resulted from the associated effects of HP-beta-CD, RGO, Nafion and in situ deposited bismuth film. Various experimental parameters such as supporting electrolytes, pH values, concentrations of Bi3+, deposition potentials and deposition times were optimized. Under the optimal conditions, the stripping currents increased linearly with increasing concentration of Pb2+ and Cd2+ in the ranges of 1 x 10(-10) to 9 x 10(-9) mol L-1 and 5 x 10(-10) to 9 x 10(-9) mol L-1,and the limit of detection (S/N = 3) were estimated to be 9.42 x 10(-11) mol L-1 for Pb2+ and 6.73 x 10(-11) mol L-1 for Cd2+, respectively. Most importantly, this developed electrochemical sensor exhibit high sensitivity, good stability and reproducibility, and will provide a superior platform in the environmental analysis and detection. (C) 2013 Elsevier Ltd. All rights reserved.