Trace level valuation of analytes by the costless method is a thriving force to construct a viable sensor. Here, the proposed norfloxacin (NFC) sensor has been developed electrochemically using nickel-cobalt metal-organic frameworks (Ni-Co-MOF) nickel foam (NF). Here, a sphere-like structure assembled with nanosheets of Ni-Co-MOF NF was obtained by a simple one-step hydrothermal synthesis. Then, to obtain ultrathin nanosheets of Ni-Co-MOF NF by immersing the obtained NF in DMF. The formation of ultrathin nanosheets was confirmed and explained by physical characterization like XRD, SEM and RAMAN studies. The prepared Ni-Co-MOF was further used to analyze the electrochemical oxidation of NFC using cyclic voltammetry and differential pulse voltammetry method with a working potential 0 to 1.25 V. Acquired DPV results at Ni-Co-MOF NF showed a respectable linear range of 0 To 69 μM, lower LOD of 0.02229 and 0.0944 μM, the higher sensitivity of 9.4 and 38.74 μA/μmol/L and reproducibility. Also, fabricated Ni-Co-MOF NF was additionally used to determine the commercially available norfloxacin tablet in urine and blood serum samples with satisfactory results.