This study introduces a new electrochemical sensor for bisphenol A (BPA) and metal ions utilizing a microsphere dual‐ligand Ni‐based MOFs modified carbon paste. The MOFs (Ni‐bipy‐btc) synthesized from dual‐ligands were prepared via a hydrothermal method and characterized using X‐ray diffraction (XRD), scanning electron microscope (SEM), FT‐IR spectrometer, X‐ray photoelectron spectrum (XPS), and specific surface area test (BET) analysis. The resulting MOFs exhibited promising performance as electrode materials for electrochemical sensors targeting the detection of BPA and heavy metal ions (Pb2+ and Cu2+). The linear range of the MOFs (Ni‐bipy‐btc)/CPE electrode for BPA detection ranged from 0.2 to 150 μM, with a detection limit of 0.045 μM, demonstrating robust immunity and stability. Additionally, the limit of detection for the MOFs (Ni‐bipy‐btc)/CPE electrode was found to be 4.3 and 9.5 nM for Pb2+ and Cu2+ ions, respectively, showcasing excellent stability and reproducibility. This study presents a straightforward approach for the highly sensitive electrochemical detection of BPA and heavy metal ions using a simple hydrothermal reaction method.