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Peroxynitrite (ONOO⁻) is a potent oxidant and nucleophile participating in a variety of pathophysiological processes as well as playing a major role in cancer therapy. However, the intracellular environment of solid tumors severely restricts the production of ONOO⁻, which leads to an unsatisfactory anticancer effect. Here, a tumor‐specific platform for ONOO⁻ generation, prepared by linking a type I photosensitizer with a GSH‐responsive NO donor, is constructed to overcome the tumor hypoxic microenvironment and enhance treatment efficiency (NBS‐2S‐NO). Responding to the overexpressed glutathione (GSH) within tumors, NBS‐2S‐NO can selectively induce ONOO⁻ generation after a cascade including red light irradiation causing superoxide radical (O₂^•−) production, GSH‐triggered NO release, and fast reaction between O₂^•− and NO. The generated ONOO⁻ can cause oxidative damage to tumor cells, induce …