Chemodynamic therapy (CDT) is a highly effective clinical treatment strategy based on the Fenton or Fenton‐like responses. However, its efficacy has been greatly limited by the complex tumor microenvironment, TME, such as the low levels of H2O2 and the overexpression of the glutathione (GSH). Polyoxometalates (POMs) are compounds that consist of anionic transition metal oxide clusters, such as tungsten (W) and molybdenum (Mo), and notably, these compounds have excellent redox properties in biological systems that can be utilized therapeutically. Therefore, POM‐CaO2@ZIF‐8 nanoparticles (NPs) have been synthesized and used as a mediator to develop an electrically enhanced CDT strategy. It is hoped that the simultaneous modulation of endogenous (the H2O2 generated by CaO2 NPs and GSH depletion by POM) and exogenous (Electric, E) stimulation enhanced Fenton‐like responses will lead to better therapeutic results. Such a treatment strategy has shown excellent tumor cell killing effects in both in vitro and in vivo studies.

Nanozymes attract widespread attention in the biomedical field owing to their catalytic activity and unique physicochemical properties, particularly for tumor catalytic therapy. Nevertheless, the complex tumor microenvironment (TME) and limited hydrogen peroxide (H2O2) restrict catalytic therapeutics by nanozymes. Enhancing the catalytic activity of nanozymes for efficient catalytic therapy is extremely meaningful for further research. Here, we report MXene-based platinum (Pt) and glucose oxidase (GOD) hybrid nanozymes (Ti3C2/Pt-GOD) for hyperthermal-enhanced cascade catalytic therapy. In this construct, the Pt nanoparticles with peroxidase-like (POD-like) and catalase-like (CAT-like) activities can catalyze H2O2 to produce reactive oxygen species (ROS) for catalytic therapy and oxygen (O2) to alleviate hypoxia simultaneously for the oxidation reaction of GOD with glucose for self-supply of H2O2. MXene as a deposition matrix coupled with photothermal properties enables photothermal therapy (PTT) and hyperthermal-enhanced catalytic therapy under near-infrared (NIR) laser. The effect of the photothermal-catalytic synergy therapy was validated both in vitro and in vivo. This construction of Ti3C2/Pt-GOD composites and hyperthermal-enhanced catalytic therapy provides a promising reference for nanozyme-mediated catalytic medicine.