In this work, a new strategy for the simultaneous determination of Pb2+ and Cd2+ was described based on amino-functionalized mesoporous silica (NH2-MCM-41) as sensing mediator. NH2-MCM-41 was prepared using a post-grafting process and the successful amino-functionality was confirmed by Fourier transform infrared (FTIR) and X-ray energy dispersive (EDS) spectra. It was found that both MCM-41- and NH2-MCM-41-modified glassy carbon (GC) electrode exhibit simultaneous response to Pb2+ and Cd2+. However, the NH2-MCM-41 modified electrode showed higher sensitivity than that of the MCM-41-modified one, which was attributed to the good chelating ability of amino groups to metal ions besides the high surface area and special mesoporous morphology of MCM-41. As a result, simultaneous assay of Pb2+ and Cd2+ was realized using anodic stripping voltammetric (ASV) method. Under the optimum experimental conditions, the linear response ranges for Pb2+ and Cd2+ ions are 0.5-250 mu gL(-1) and 50-450 mu gL(-1), respectively. The corresponding detection limits are 0.2 mu gL(-1) for Pb2+ and 1.0 mu gL(-1) for Cd2+, with good electrode renewability, which is defined as the complete removal of the accumulated metals from the electrode surface. In addition, the NH2-MCM-41 modified electrode was demonstrated for the successful determination of Pb2+ and Cd2+ in real samples, including tap water, lake water and tea. (C) 2014 Elsevier Ltd. All rights reserved.