In this study, a novel process for synthesizing ZnO nanoparticles using a non-thermal plasma source generated by the Gliding Arc Discharge (GAD) system is presented. The physicochemical properties of the synthesized nanoparticles were characterized using diverse techniques such as scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), UV-Visible spectroscopy (UV-Vis), Fourier transforms infrared spectroscopy (FTIR), and X-ray diffraction (XRD). Furthermore, the effectiveness of the synthesized ZnO nanoparticles for wastewater treatment was evaluated by testing their photocatalytic activity against Brilliant Cresyl Blue (BCB) and Congo Red (CR) using UV light irradiation for 2 hours and 30 minutes. The results confirmed the successful synthesis of highly pure spherical ZnO nanoparticles with a size of 27.18 nm and band gap energy of 3.30 eV in an extremely short duration and simple steps. Furthermore, the GAD plasma-assisted ZnO nanoparticles showed a significant dye removal rate of 90%, demonstrating their potential as a highly effective material for photocatalytic wastewater treatment. This study provides new insights into the application of GAD plasma for nanoparticle synthesis.