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Fullerene has shown great potential both in drug delivery and photodynamic therapy. Herein, we developed a doxorubicin (DOX)-loaded poly(ethyleneimine) (PEI) derivatized fullerene (C60–PEI–DOX) to facilitate combined chemotherapy and photodynamic therapy in one system, and DOX was covalently conjugated onto C60–PEI by the pH-sensitive hydrazone linkage. The release profiles of DOX from C60–PEI–DOX showed a strong dependence on the environmental pH value. The biodistributions of C60–PEI–DOX were investigated by injecting CdSe/ZnS (Qds) labeled conjugates (C60–PEI–DOX/Qds) into tumor-bearing mice. C60–PEI–DOX/Qds showed a higher tumor targeting efficiency compared with Qds alone. Compared with free DOX in an in vivo murine tumor model, C60–PEI–DOX afforded higher antitumor efficacy without obvious toxic effects to normal organs owing to its good tumor targeting …