Cobalt zinc-zeolite imidazole framework (Co/Zn-ZIF) nanofibers are made via an electrospinning (ES) approach and tested for the detection of heavy metal cadmium ions. Electrostatically attracted cobalt and zinc ions are bound regularly on the surface of the ZIF network. The cobalt and zinc ions are organized with the ZIF network, which provides the sturdily bonded tetrahedral structure of Co/Zn-ZIF, giving essential steadiness to the composite material. Cyclic voltammetry revealed that the observed profile is reversible, and the catalytic behavior of the electrodes provided evidence of interfacial electron transfer between the nanofiber-modified GCE surface and the metal ions. Interestingly, a careful determination of Cd2+ ions within the range of 100 nM to 1 mM with a low limit detection of 27.27 nM was undertaken. The established heavy metal ion detector shows excellent anti-interference abilities toward the observed electroactive species, and it was successfully employed using a tap water sample for Cd2+ ion detection, where good results were observed.