LAUSR

Tumor microenvironment (TME)‐activated cancer imaging and therapy is a key to achieving accurate diagnosis and treatment of cancer and reducing the side effects. Herein, smart near‐infrared carbon dot‐metal organic framework MIL‐100 (Fe) assemblies are constructed to achieve TME‐activated cancer imaging and chemodynamic‐photothermal combined therapy. First, a near‐infrared emission carbon dot (RCDs) is developed using glutathione (GSH) as the precursor. Then, the RCDs@MIL‐100 self‐assemblies are obtained using RCDs, FeCl3, and trimesic acid solutions as raw materials. After the RCDs@MIL‐100 enters the TME, a high concentration of GSH reduces Fe3+ to Fe2+ and drains the GSH, triggering the collapse of RCDs@MIL‐100 skeleton and the release of RCDs and Fe2+, at which time the RCDs fluorescence is restored and in an “on” state to illuminate the tumor cells, which achieved cancer imaging. The released Fe2+ reacts with H2O2 in the TME to form highly reactive hydroxyl radicals (•OH) by Fenton reaction, which achieves the chemodynamic therapy of tumors. Thus, efficient synergistic chemodynamic‐photothermal dual mode therapy is achieved under fluorescence imaging guidance with TME response.