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It is essential for developing an effective and accurate method for analysis for detecting 4-nitrophenol (4-NP), as its harmful effect is one of the most frequent environmental concerns. In this work, the 4-NP was detected by the CNF/CZO nanocomposite. The cobalt-doped zinc oxide (CZO) was synthesized utilizing a simple hydrothermal technique and carbon nanofiber (CNF) was combined with cobalt-doped zinc oxide (CZO) to get CNF/CZO nanocomposite. The morphological and chemical characteristics of the CNF|CZO nanocomposite have been studied using several characterization techniques. The CZO nanoparticles have equal dispersion across the surface of the CNF and the nanocomposites were modified with a glassy carbon electrode (GCE), which is utilized as a working electrode for the electrochemical studies. Hence, the CNF|CZO the nanocomposite was confirmed using field emission scanning electron microscopy, Transmission Electron Microscopy, Energy Dispersive X-ray analysis, X-ray Diffraction Analysis, and X-ray Photoelectron Spectroscopy, Fourier-transform infrared spectroscopy, Electrochemical Impedance Spectroscopy, Cyclic Voltammetry research, and Differential Pulse Voltammetry studies were done. Hence, the GCE|CNF|CZO electrode displays a low detection limit of 0.2 μM, a wide linear response range of 0.01–520 µM, and a higher sensitivity of 0.0137 μA μM−1 cm−2. Further, the GCE|CNF|CZO electrode detected 4-NP in environmental water samples and also showed exceptional selectivity, repeatability, stability, and reproducibility. Hence, we conclude that GCE|CNF|CZO electrode exhibited good catalytic activity due to the inherent interaction between CNF and CZO providing an electron transfer network and high catalytic activity towards 4-NP detection. [Display omitted] • The GCE|CNF|CZO electrodes applied for the detection of 4-NP in environmental water samples. • Cobalt-doped Zinc Oxide (CZO) was synthesized by hydrothermal method. • The GCE|CNF|CZO exhibited 4-NP detection limit was LOD of 0.2 μM with wide linear response range of 0.01-520 µM. • The electrode sensitivity was identified as 0.0137 µA µM−1 cm−2. • The practical applicability of the electrode was tested in environmental water samples. [ABSTRACT FROM AUTHOR]