Metal-organic framework (MOF) materials exhibit unique advantages in adsorption, pre-enrichment and selective recognition of heavy metal ions due to their porous nature, tunable structure and ease of functionalization. However, due to the poor conductivity and electrochemical activity of most MOFs, their application in electrochemical sensing is limited. In this paper, an electroactive hybrid material rGO/UiO-bpy composed of UiO-bpy and electrochemically reduced graphene oxide (rGO) was prepared and has been successfully used in the electrochemical determination of lead ions (Pb2+). Interestingly, a reverse response relationship between the electrochemical signal of UiO-bpy and the concentration of Pb2+ was discovered in the experiment, which can be used to develop a novel on-off ratiometric sensing strategy for Pb2+ detection. To our knowledge, this is the first time that UiO-bpy has been used as both an improved electrode material for heavy metal ion detection and an internal reference probe for ratiometric analysis. This study is of great significance to expand the electrochemical application of UiO-bpy and develop innovative electrochemical ratiometric sensing strategies for Pb2+ determination.