A. G. Bindu, Ramesh S. Bhat
4‐aminophenol (AMP) and 4‐acetamidophenol (ACP) are significant compounds in the pharmaceutical, dye, and cosmetic industries and analytical fields, with the uncontrolled release caused serious of environmental and health risks. So, necessitating their sensitive and selective detection through voltammetric studies. To achieve this, Chromium Titanium Yttrium oxide nanocomposites (CrTiYONC) were synthesised via a simple combustion method using chromium(III) nitrate, titanium(III) nitrate, and yttrium(III) nitrate as precursors, with glycine serving as the fuel. The combustion process is carried out at 750°C, producing phase‐pure nanostructures. These nanocomposites are then employed to modify the electrode surface, where an arginine‐functionalized polymeric film was electrochemically deposited onto the carbon paste electrode through the cyclic voltammetric technique. The modified electrode displays an enhanced active surface area, better conductivity, and augmented transfer of electron–proton owing to the synergistic effect of CrTiYO NC structures and the polymeric film. The electrochemical studies, like electrochemical impedance spectroscopy, cyclic voltammetry, linear sweep voltammetry, and differential pulse voltammetry, disclose that the AM‐CrTiYO‐CPE follows a diffusion‐controlled electrochemical redox mechanism with optimised conditions of 0.1 M BS solution at pH 7.2 in 0.1 V s −1 scan rate. The developed AM‐CrTiYO‐CPE validates remarkable electrocatalytic activity toward the detection of AMP and ACP, achieving low detection limits in a wide linear range. The fabricated electrode further displays an excellent stability, selectivity, sensitivity, reproducibility, and repeatability, with kinetics and availability of the electroactive site. The selective nature of the AM‐CrTiYO‐CPE electrode toward the quantification of AMP and ACP highlights its significant potential for applications in pharmaceutical formulation analysis, enironmental monitoring, drug delivery systems, quality control, and clinical diagnostics.