In Vivo X‐ray Triggered Catalysis of H 2 Generation for Cancer Synergistic Gas Radiotherapy

To date, hydrogen (H 2 ) therapy has received widespread attention. However, X‐ray triggered sustainable H 2 ‐producing materials with controlled release for cancer treatment have not been reported. Herein, an X‐ray triggered sustainable in situ H 2 producing platform, Au NR‐TiO 2 @ZnS:Cu,Co‐A(Au‐TiO 2 @ZnS), composed of Au‐amorphous TiO 2 nano‐dumbbell‐shaped heterostructure coated with long afterglow particles, was developed for cancer synergistic H 2 ‐radiotherapy. The mechanism of H 2 production was verified by theoretical calculations and in vitro experiments. Changes in the apoptosis pathway caused by the synergistic effect of H 2 and radiotherapy were reported. Guided by its excellent photoacoustic imaging capabilities, mice with orthotopic liver cancer achieved excellent therapeutic effects and low inflammatory side effects, suggesting that Au‐TiO 2 @ZnS has promising application potential for cancer treatment and prognosis.