Abstract: Au/TiO2 nanocomposite particles were synthesized by a method based on intense X-ray irradiation without adding any reducing agent or stabilizer. The nanocomposite exhibits promising photocatalytic and biological properties at physiologically relevant concentration ([Au] = 0.028 mM, [TiO2] = 0.5 mM). The structure and photocatalysis were examined by X-ray diffraction, electron microscopy and ultraviolet–visible spectroscopy demonstrating that gold nanoparticles of 2–5 nm size were successfully deposited on TiO2 nanoparticle surfaces. The nanocomposite exhibited good colloidal stability within a typical cellular environment and was nontoxic to cancer cell according to evaluations under controlled conditions. The Au/TiO2 nanoparticles were also found to enhance the photocatalytic efficiency of UV radiation and even more that of X-ray radiation. In vitro studies indicated that the cell-killing effect under X-ray irradiation is more pronounced with the addition of Au/TiO2 nanoparticles than of bare TiO2 nanoparticles.