This paper reports the synthesis and characterization of a graphene oxide-gold nanohybrid (GO-Au) and evaluates its suitability as a test material, e.g., in nano(eco)toxicological studies. In this study, we synthesised graphene oxide (GO) and used it as a substrate for the growth of nano-Au decorations, via the chemical reduction of gold (III) using sodium citrate. The GO-Au nanohybrid synthesis was successful, producing AuNPs (~17.09 ± 4.6 nm) that were homogenously distributed on the GO sheets. They exhibited reproducible characteristics when characterised using UV-Vis, TGA, TEM, FTIR, AFM, XPS and Raman spectroscopy. The nanohybrid also showed good stability in different environmental media and its physicochemical characteristics did not deteriorate over a period of months. The amount of Au in each of the GO-Au nanohybrid samples was highly comparable, suggesting a potential for use as chemical label. The outcome of this research represents a crucial step forward in the development of a standard protocol for the synthesis of GO-Au nanohybrids. It also paves the way towards a better understanding of the nanotoxicity of GO-Au nanohybrid in biological and environmental systems.