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Hypoxia is one of the major factors that affect the efficiency of photodynamic therapy (PDT). However, the strategy of using nano‐oxygen carriers to reverse tumor hypoxia still has some drawbacks, which limit its clinical application and translation. Herein, it is reported a method for preparing pH‐sensitive nano‐oxygen carrier for reversing tumor hypoxia and enhancing the efficiency of PDT. Briefly, perfluorocarbons (PFC) with different chain‐lengths (7F or 15F) are linked by acid‐labile ortho ester bonds, then further self‐assembled with Chlorin e6 to form two pH‐sensitive nanodrugs. In vitro tests demonstrate that these nanodrugs possessed good physicochemical properties, including high stability, anti‐adsorption capability, and high oxygen‐loading capacity (24.5 mg L−1). In vivo studies reveal that this system can remarkably alleviate tumor hypoxia and inhibit tumor growth, and 15F@OE dimer particles display the highest antitumor efficiency (84.2%). Overall, this study presents a simple and efficient strategy to deliver oxygen and drugs to tumor tissue, thereby overcoming the limitation of hypoxia‐mediated PDT in cancer treatment.

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