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[Display omitted] • A multi-layer architecture of NiMOFs was synthesized and characterized by SEM, XRD, XPS, Raman, IR, and EIS. • The insertion of helical-shaped MWCNTs into NiMOFs has been done for enhanced electrocatalytic sensing applications. • The surface adsorption efficiency of the different modified electrodes was discussed. • The designed binder-free (GCE/MWCNT@NiMOFs) electrochemical probe exhibited a satisfactory limit of detection and wide linear response. • The designed electrochemical probe was successfully employed in real-world samples and achieved excellent recovery ranges with high reproducibility. Nitroimidazole-based drugs are widely used as an antibiotic for the treatment of anaerobic bacterial and parasite illnesses. The widespread use of these drugs in animal feed and the consequent environmental pollution have become significant concerns in recent years. Simple, sensitive, and rapid detection of the antibody in various real samples is demanding research interest. Herein, we report a Nickel-metal organic framework functionalized Multiwalled Carbon nanotubes modified glassy carbon electrode (MWCNT@NiMOFs) as an ultrasensitive and rapid voltammetric sensor for the detection of ornidazole (ORDZ) in a neutral pH solution. The MWCNT@NiMOFs were prepared using a microwave-assisted solvothermal technique accompanied by an ultrasonication method. The designed MWCNT@NiMOFs offered a low charge transfer resistance (R ct) of 141 Ω along with excellent electrocatalytic activity, and high current density at the lowered cathodic peak potential (-0.62 V vs Ag/AgCl) for ORDZ detection. The surface adsorption capacity (Γ s) in terms of surface excess and heterogeneous charge transfer rate constant (k 0) of the MWCNT@NiMOFs were calculated to be 3.29 × 10-9 mol cm−2 and 5.33 × 10-3 cm s−1, respectively. Under an optimal working condition, differential pulse voltammetry measurements of ORDZ have shown concentration linearity in a window, 100 nm to 10 µM range with excellent sensitivity, 5.69 × 10-5A µM−1 cm−2, and detection limit, 26 nM (3.3/s). The designed MWCNT@NiMOFs offered appreciable reproducibility, and repeatability up to 30 days of storage time. The real-time quantitative evaluation of ORDZ in human urine and tap water specimens was done along with ∼ 100 % recovery values. Since the new approach is simple, selective, and separation-free, it can be extendable to a variety of real-time practical applications. [ABSTRACT FROM AUTHOR]