• NiO@Gd 2 O 3 was synthesized via the facile co-precipitation method. • Modified sensor were studied by CV and DPV techniques for TRH detection. • NiO@Gd 2 O 3 electrode displayed WLR, low LOD, and excellent sensitivity. • The fabricated sensor shows good selectivity in MT, DA, UA, and CPZ towards TRH. The construction of mixed metal oxides matrix acts as highly active electrode materials in the field of an electrochemical sensor, owing to high conductivity, a large number of active sites, fast kinetics, and superior sensing activity. In this study, the spherical-like NiO@Gd 2 O 3 (NGO) microstructures were successfully synthesized by a simple co-precipitation method and employed for the selective electrochemical detection of thioridazine hydrochloride (TRH). The as-prepared NGO-500 material was confirmed with suitable spectrometric techniques such as X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Raman spectroscopy, Brunauer–Emmett–Teller (BET) method, field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectrometry (XPS) analyses. The electrocatalytic performance of TRH on modified screen-printed carbon electrode (NGO-500/SPCE) was investigated through cyclic voltammetric (CV), and differential pulse voltammetric (DPV) methods. As a result, the proposed electrode demonstrated a wide linear response of 0.04–151.6 µM, a low detection limit of 0.004 µM with an excellent sensitivity of 3.09 µA µM −1 cm −2 . Besides, the modified electrode establishes outstanding selectivity in the presence of the various interfering compounds towards TRH detection. The fabricated electrode displayed notable repeatability, reproducibility, acceptable cyclic and storage stability. The feasibility of the NGO-500 electrode was used to sense TRH in urine and serum samples with satisfactory results.
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