The necessity for highly sensitive and precise methodologies for monitoring water quality and safety is imperative. The substantial health risks linked with Nhydroxysuccinimide (NHS) in water samples and its contact with the skin and eyes are noteworthy. Despite the utilization of numerous techniques for NHS analysis, the adoption of a rapid and uncomplicated electrochemical process has been infrequent. This article details the fabrication of an electrochemical NHS detection system using a cerium zirconium oxide (CZO)-doped reduced graphene oxide (rGO) nanocomposite. The CZO/ rGO nanocomposite was prepared through a straightforward method involving precipitation and sonication. Structural analysis of the CZO/rGO involved various techniques, including X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), Raman spectroscopy, field emission scanning electron microscopy (FE-SEM), elemental mapping, energy dispersive X-ray analysis (EDX), and X-ray photoelectron spectroscopy analysis (XPS). Crucial kinetic parameters, such as the effective surface area, were evaluated for CZO/rGO on the glassy carbon electrode (GCE). Additionally, the CZO/rGO/GCE showcased reduced charge transfer resistance (R ct = 99 Ω), exceptional electrochemical activity, a high electron transfer rate, and strong selectivity. This electrode demonstrated excellent electrochemical sensing capabilities for NHS, boasting an extremely low detection limit (0.045 μM) and heightened sensitivity of 0.020 μA μM −1 cm −2 . Demonstrating its potential for swiftly detecting NHS in river water, the CZO/rGO/GCE sensor achieved over 97% recovery. This approach is particularly well-suited for creating water pollution sensors in various sensing devices.