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A nanostructured material of the type Au-ZnO-SiO is described that consists of ZnO and gold nanoparticles (NPs) dispersed into a silica matrix and used to construct a voltammetric sensor for 4-nitrophenol. The AuNPs and ZnO NPs are anchored onto the silica network which warrants the nanostructures to be stable in various environments. It also facilitates the electron transfer between the electrolyte and the glassy carbon electrode (GCE). The properties of the nanostructure as a modifier for the GCE were investigated by energy dispersive spectrometry, X-ray diffraction spectroscopy, and transmission electron microscopy. It is shown that the nanostructure increases the surface area. Hence, the cathodic and anodic current in differential pulse voltammetry of 4-nitrophenol are considerably enhanced in comparison to a bare GCE. Under optimum conditions, the currents for oxidation and reduction are proportional to the concentration of 4-nitrophenol in the 0.05-3.5 μM and 0.01-1.2 μM concentration ranges, with 13.7 and 2.8 nM detection limits, respectively. The sensor has excellent sensitivity, fast response, long-term stability, and good reproducibility. It is perceived to be a valuable tool for monitoring 4-nitrophenol in real water samples. Graphical abstract Schematic of voltammetric sensor for 4-nitrophenol. It is based on GCE modified with gold-ZnO-SiO nanostructure. It exhibited the improvement in performance for both oxidation and reduction peaks in terms of linearity, concentration range, detection limit, and sensitivity.