Green synthesis of NiSnO3 nanopowder was carried out via chemie douce using nickel and tin chlorides as precursors by stirring and refluxing at 80 ℃. The dried dark green bimetallic oxide nanoparticle was then used for preparing the sensing electrode in the form of a screen-printed electrode (SPE). The synthesized nanoparticles were analyzed for elemental, structural, and morphological characteristics using various analytical techniques. The Fourier transform infrared (FTIR) spectrum indicated the formation of a strong Sn–O–Ni framework, while X-ray diffraction (XRD) confirmed the formation of a bimetallic oxide nanopowder of NiSnO3. The synthesized nanoparticles were studied for hydroquinone (HQ) sensing characteristics to develop a sensitive and reproducible electrochemical sensor from 1 to 9 mM concentrations in buffer. The developed sensor exhibited a sensitivity of 6.03 µA/mM (46.38 µA/mMcm−2). The charge transfer studies indicated a reversible and diffusion-controlled process. To the best of our knowledge, such a material, i.e., NiSnO3, has not be used for HQ sensors and is being reported for the first time.