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Abstract Pyroptosis possesses potent antitumor immune activity, making pyroptosis inducer development a promising direction for tumor immunotherapy. Persistent luminescence nanoparticles (PLNPs) are highly sensitive optical probes extensively employed in tumor diagnosis and therapy. However, a pyroptosis inducer based on PLNPs has not been reported yet. Herein, polyethylene glycol–poly lactic acid‐co‐glycolic acid (PEG–PLGA: PP) modified biodegradable CaS:Eu2+ (CSE@PP) PLNPs are synthesized as a pyroptosis inducer for tumor immunotherapy for the first time. The synthesized CSE@PP possesses biowindow persistent luminescence (PersL) and pH‐responsive degradation properties, allowing it to remain stable under neutral pH but degrade when exposed to weak acid (pH < 6.5). During degradation within the tumor, CSE@PP constantly releases H2S and Ca2+ while its PersL gradually fades away. Thus, the PersL signal can self‐monitor H2S and Ca2+ release. Furthermore, the released H2S and Ca2+ result in mitochondrial dysfunction and the inactivation of reactive oxygen species scavenging enzymes, synergistic facilitating intracellular oxidative stress, which induces caspase‐1/GSDM‐D dependent pyroptosis and subsequent antitumor immune responses. In a word, it is confirmed that CSE@PP can self‐monitor H2S and Ca2+ release and pyroptosis‐mediated tumor Immunotherapy. This work will facilitate biomedical applications of PLNPs and inspire pyroptosis‐induced tumor immunotherapy.

Near-infrared (NIR) persistent luminescence nanoparticles (PLNPs) have inherent advantages for high-sensitivity bioimaging due to the separation of excitation and emission light. However, the single-wavelength emission of NIR PLNPs for bioimaging limits their use in photodynamic therapy (PDT). Herein, a biological window excited up-conversion (UC) PLNPs, Zn3Ga2SnO8:Cr3+,Yb3+,Ho3+ (ZGS), was reported for bioimaging and PDT. ZGS exhibits NIR persistent luminescence (PersL) after red LED excitation and visible UCL under 980 nm excitation. The NIR PersL is designed for in vivo bioimaging; the visible UCL is used to activate photosensitizer (PS) to generate reactive oxygen species (ROS) for PDT. The dual-functional ZGS with UCL and PersL provides an effective method for bioimaging and PDT, which is expected to further promote the application of PLNPs in the integration of efficient diagnosis and treatment.