Hypoxic and acidic environments are the two main components of the microenvironment contributing to the poor efficacy of chemotherapy drugs in the treatment of oral squamous cell carcinoma (OSCC). In this study, we synthesized a series of Zn1-x Mg x Fe2O4 nanomaterials with enzyme-like properties, including catalase (CAT)-like, peroxidase (POD)-like, and glutathione (GSH)-like activity in an acidic environment. Among them, Zn0.4Mg0.6Fe2O4 performed the best and effectively increased the efficacy of doxorubicin (DOX) chemotherapy for the treatment of OSCC with reduced cardiotoxicity. Therefore, Zn0.4Mg0.6Fe2O4 could serve as a novel chemosensitizer in the treatment of OSCC.
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