In this study, the phosphidation of zirconium phosphate nanoparticles (ZrP) was pursued to create zirconium phosphide on the surface of ZrP (ZrP@P) by the calcination process. The morphology and structure of prepared ZrP and ZrP@P were characterized by different methods including XPS, SEM, XRD, and FT-IR. Deposited nanocomposite on a glassy carbon electrode (ZrP@P/GCE) showed boosted electrochemical properties towards oxidation of Asulam investigated by cyclic and differential pulse voltammetry techniques. After optimizing the variables affecting the ZrP@P/GCE response, the Asulam quantification was tested, and the linear range of 5–45 µg/L and detection limit of 0.16 µg/L were obtained. The phosphidation process increased the surface-active points and the active surface area of the ZrP facilitating the interaction of Asulam molecules with the GCE surface modified with ZrP@P. The ZrP@P/GCE accurately quantified Asulam in real samples such as tomato, lettuce, and cucumber with obtained recovery values of 96–113% and RSD≤4.4%. This sensor offers a simple, low-cost, and convenient method to detect Asulam
