In this paper, we constructed MIL-53 (AlOHbdc, bdc = benzene-1,4-dicarboxylate) /CNTs and Prussian blue (PB) as the double sensitization material of the sensing platform, in which the MIL-53/CNTs hybrid can not only increase the specific surface area but also increase the conductivity of the sensor and PB can play a role in amplifying electrical signals and accelerating electron transmission. Pyrrole was used as monomer and E2 was used as template for electropolymerization to form conductive film. Moreover, the overoxidation/dedoping elution method were used to simplify the experimental process. Under optimal conditions, the MIECS exhibited an excellent sensitivity and high selectivity with a wide linear response range between 10 to 10 mol L and an estimated detection limit of 6.19 × 10 mol L.