In this study, for the first time, a selective electrochemical sensor by glassy carbon electrode (GCE) modified with the covalent organic framework (COF) and carbon black (CB) was introduced and applied to simultaneous sensing of Zn2+, Cd2+, Pb2+, and Hg2+ via differential pulse anodic stripping voltammetry (DPASV). The COF is supplied through a condensation reaction between melamine and trimesic acid. The COF and CB, which are used to modify the GCE surface, increase electrochemical activity. The linearity to determine ions was achieved as Zn2+: 0.009–1100 nM, Cd2+: 0.005–1100 nM, Pb2+: 0.003–1100 nM, and Hg2+: 0.001–1100 nM. Besides, the detection limits for Zn2+, Cd2+, Pb2+, and Hg2+ have obtained 0.003, 0.002, 0.001 and 0.0003 nM, respectively. The CB-COF/GCE was applied to simultaneously measure the ions in food samples. For validation, atomic absorption spectrometry (AAS) was applied to measure the amount of target metal ions as a standard method in real samples.
