In this study, well-dispersed gold nanoparticles were prepared by the reduction of HAuCl4 in sodium bis(2-ethylhexyl)sulfosuccinate/isooctane reverse micelles system using ascorbic acid as reducing agent. The properties of the obtained nanoparticles were characterized with transmission electron microscopy, X-ray diffraction, thermogravimetric analysis, and UV-vis absorption spectrophotometer. Due to its high water solubility, biodegradability, and low toxicity, ascorbic acid could be used as a benign naturally available reducing agent to synthesize gold nanoparticles.