In this paper,graphene(rGO) was immobilized on the surface of the electrode by the method of electrochemical reduction of graphene oxide(GO),and then the copper hydroxide-nickel hydroxide nanocomposites were electrodeposited to form graphene/metal hydroxide nanocomposites modified glassy carbon electrode(GCE/rGO/Cu(OH)2-Ni(OH)2).Finally,horseradish peroxidase(HRP) was immobilized onto the surface of the above prepared electrode by electropolymerizing azure I to form the GCE/rGO/Cu(OH)2-Ni(OH)2/HRP-PA(PA: poly azure Ⅰ).The graphene/metal hydroxide nanocomposites were characterized by SEM and EDS.The preparation process and electrochemical performance of the sensor were investigated by electrochemical impedance spectroscopy and cyclic voltammetry.Hydrogen peroxide tert-butyl(BHP) and cumene hydroperoxide(CHP) were determined by the sensor.The linear response of the HRP sensor to BHP was in the concentration range of 2.0×10-5-9.2×10-4mol/L with a detective limit of 9.9×10-6mol/L and that to CHP was in the concentration range of 3.0×10-6-1.0×10-4mol/L with a detective limit of 6.9×10-7mol/L.