A new type of electrochemical sensor based on multi-walled carbon nanotubes(MWCNTs), K2H4SiW11CuO39·6H2O(SiW11Cu) and gold nanoparticles(AuNPs) was prepared for the simultaneous detection of bisphenol A and acetaminophen. Differential pulse voltammetry(DPV), cyclic voltammetry(CV) and electrochemical impedance spectroscopy(EIS) were used for electrochemical characterization, and Fourier transform infrared spectroscopy(FTIR) was used to characterize the structure of polyoxometalates. Electrochemical experimental results show that the composite modified electrodes have good electrochemical activity as well as current response values of bisphenol A and acetaminophen when pH=7.0. At the same time, the modified electrode exhibits good stability and reproduction, and has good anti-interference ability to other substances. In practical application, the sensor obtained satisfactory results.