Gold nanoparticles were prepared by metal-vapor synthesis using isopropanol, acetone or toluene as dispersion media. The electronic states of the metal and the nature of the sorbed layer on the surface of the nanoparticles were studied. The analysis of photoelectron spectra of the obtained nanoparticles showed that regardless of the synthesis conditions, gold in all samples is in the Au0, Au+ and Au3+ states and a carbon-containing shell is present on all types of metal particles. The study of anticancer activity of nanoparticles in vitro with human cell lines showed the dependence of biological activity on their interaction time of samples obtained in toluene dispersion medium. The metabolic activity of gold nanoparticles obtained in isopropanol or acetone medium decreased in the earliest period of testing.