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Sonodynamic therapy (SDT) typically suffers from compromised anticancer efficacy owing to the low reactive oxygen species (ROS) yield and complicated tumor microenvironment (TME) which can consume ROS and support the occurrence and development of tumors. Herein, ultrathin‐FeOOH‐coated MnO2 nanospheres (denoted as MO@FHO) as sonosensitizers which can not only facilitate ultrasound (US)‐triggered ROS but also tune the TME by hypoxia alleviation, H2O2 consumption as well as glutathione (GSH) depletion are designed. The FeOOH coating will boost the production yield of singlet oxygen (1O2) and hydroxyl radicals (•OH) by inhibiting the recombination of US‐initiated electron–hole pairs and Fenton‐like reaction, respectively. Additionally, the catalase‐like and GSH peroxidase‐like activities of MO@FHO nanospheres enable them to break the TME equilibrium via hypoxia alleviation and GSH depletion. The combination of high ROS yield and fundamental destruction of TME equilibrium results in satisfactory antitumor outcomes, as demonstrated by the high tumor suppression efficacy of MO@FHO on MDA‐MB‐231‐tumor‐bearing mice. No obvious toxicity is detected to normal tissues at therapeutic doses in vivo. The capability to modulate the ROS production and TME simultaneously can afford new probability for the development of advanced sonosensitizers for synergistic comprehensive cancer therapy. [ABSTRACT FROM AUTHOR]

Intraoperative diagnosis of metastatic tumors is of significant importance to the treatment of ovarian cancer. NIR‐II fluorescence imaging holds great promise for facile detection of tumor in situ with high sensitivity and resolution. Herein, a kind of NIR‐II fluorescent polymer dots (NIR‐II Pdots) with high brightness is developed for real‐time detection of metastatic ovarian cancer via NIR‐II fluorescence imaging. The NIR‐II Pdots are constructed via the self‐assembly of NIR‐II emissive aggregation induced emission luminogens (NIR‐II AIEgens) and poly (styrene)‐graft‐poly(ethylene glycol) in water. Such NIR‐II Pdots show very high fluorophore contents of nearly 30% and high quantum yield of 5.4% at emission maximum near 1020 nm. Further modification of the NIR‐II Pdots with targeting peptides yields NIR‐II Pdots‐GnRH, which can afford enhanced affinity of NIR‐II Pdots to ovarian cancer. Upon intravenous injection of the NIR‐II Pdots, whole‐body organs and vessels, peritoneal and lymphatic metastases of ovarian cancer are clearly visualized by NIR‐II fluorescence imaging. Under the guidance of NIR‐II fluorescence imaging, the metastatic foci with the diameter down to ≈2 mm can be facilely eliminated. The results indicate preclinical potential value of the NIR‐II Pdots for metastatic ovarian cancer detection. [ABSTRACT FROM AUTHOR]