Easy and mass preparation of highly efficient single atomic electrocatalysts (SAECs) for wide applications in constructing sensitive electrochemical sensing remains a great challenge. In this work, a heterogeneous SAEC was synthesized by dispersing the copper phthalocyanine (CuPc) molecular on porous Ce-BTC for sensitive, simultaneous detection of NO2- and Bisphenol A (BPA) in water. Herein, CuPc has a typical Cu-nitrogen-carbon (Cu-N4) conjugated structure and highly efficient single-atom catalytic sites with excellent catalytical efficiency and conductivity, while Ce-BTC exhibited adsorption and activation of NO2- and BPA, as well as provided matrix to better disperse CuPc to obtain Cu-N4/Ce-BTC heterogeneous catalysts. Thus, the synergistic effect of CuPc and Ce-BTC enables Cu-N4/Ce-BTC to have a highly efficient catalytic activity and stability. Impressively, the coordinated carbon and nitrogen atoms surrounding the Cu help in activating pollution molecules, which can further enhance the sensitivity. As a result, the Cu-N4/Ce-BTC sensor for detecting NO2- and BPA exhibited good stability, reproducibility, selectivity, and a wide linear range of 20-1000 μM and 10-1000 μM with a low detection limit of 0.5 and 0.15 μM, respectively. This research presents a simple and mass product synthesizing SAECs approach, which will promote the development of SAEC applications in electrochemical sensors.