The studies on the reduction of Au 3+ to gold nanoparticles in presence and absence of Cu 2+ under deoxygenated conditions in 2-propanol by radiolytic method have been carried out. On γ-radiolysis, preliminary yellow colored solution of Au 3+ changed to purple color owing to gold nanoparticles formation, which exhibits an absorption peak at around 540 nm. In the presence of Cu 2+, absorption of gold–copper nanoparticles, which was also produced during γ-radiolysis, was red shifted in contrast to the system containing no Cu 2+. Under DLS studies the sizes of gold nanoparticles in the absence and the presence of Cu 2+ were found to be larger (>400 nm). However, in presence of polyethylene glycol, a stabilizer the nanoparticle sizes became smaller, sizes measured for gold and gold–copper nanoparticles are 40 and 140 nm, respectively. Moreover, the change in UV–vis spectra in the Cu 2+ and Au 3+ mixed system highlights the formation of gold–copper nanoparticles in core–shell type arrangement.