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We report on strong X-ray-induced hydroxyl radical (.    O H    ) generation in an aqueous solution containing UV light pre-treated GdYVO4:Eu3+ nanoparticles (L-GdYVO). The methods of optical spectroscopy were used to detect .    O Hin the solutions. The complex nature of the mechanism of .    O Hgeneration has been revealed and discussed. The experimental data obtained indicate that the mechanism of .    O Hgeneration is associated with two main processes: (i) direct .    O Hgeneration with the participation of thermalized h+ formed at X-ray irradiation, and (ii) X-ray-facilitated jumps of h+ formed in the nanoparticles’ (NPs’) valence band at UV light pre-treatment and trapped in local levels formed by random scattering potential. At the same time, for GdYVO4:Eu3+ nanoparticles, which were not exposed to UV light before the X-ray irradiation (D-GdYVO), a strong radioprotective effect ascribed to the electron-donation properties of V4+ ions was observed. Thus, depending on the pre-treatment condition, we can change the redox properties of GdYVO4:Eu3+ NPs in an opposite direction, which makes this nanomaterial a unique theranostic agent for radiation therapy (RT) enhancement, allowing the problem of radiation therapy (RT)-resistant hypoxic tumours to be overcome.

X-ray Induced Hydroxyl Radical Generation by GdYVO4:Eu3+ Nanoparticles in Aqueous Solution: Main Mechanisms