Plasma applications are widely used in a wide variety of processes in materials science and technologies. Gas-phase plasma and solid-phase plasma are useful and are developed for many technologies, such as coating, production of electronic devices, surface treatment, and nanomaterial synthesis. On the other hand, the solution plasma technique is a kind of electrohydrodynamic discharge technique and has recently been studied for potential applications in plasma physics. In this study, gold nanoparticle synthesis was performed by solution plasma technique. Electrohydrodynamic discharge was created with a bipolar DC power source (15 kHz–1.6 kV–2 μs) in a 0.86-mM aqueous chloroauric acid solution. The characteristic of the plasma formed was performed by optical emission spectrometry, and the characteristics of the aliquots taken from the reaction environment at specific time intervals were also performed by UV, XRD, and FESEM analysis. As a result, gold nanoparticles were obtained with atomic sizes ranged from 30 to 50 nm.