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Contrast agents for bioimaging suffer from low accumulation at lesion area and high uptake in the reticuloendothelial system (RES). Assembly of nanoparticles in vivo improves their enrichment at tumors and inflamed areas. However, uncontrollable assembly also occurs at the liver and spleen owing to the uptake of nanoparticles by the RES. This is known to probably cause a higher bioimaging background and more severe health hazards, which may hamper the clinical application. Herein, a new near‐infrared (NIR)‐controlled supramolecular engineering strategy is developed for in vivo assembly and disassembly between lanthanide upconversion nanoparticles and second near‐infrared window (NIR‐II, 1000–1700 nm) nanoprobes to realize precision bioimaging of tumors. A supramolecular structure is designed to realize assembly via host–guest interactions of azobenzene and β‐cyclodextrin to enhance the retention of NIR‐II nanoprobes in the tumor area. Meanwhile NIR‐laser‐controllable nanoprobes disassembly brings about a reduction in the bioimaging background as well as acceleration of their RES clearance rate. This strategy may also be used in other nano‐to‐micro‐scale contrast agents to improve bioimaging signal‐to‐noise ratio and reduce long‐term cytotoxicity.
A near‐infrared (NIR)‐light‐controlled supramolecular engineering strategy is developed for in vivo assembly and disassembly between lanthanide upconversion nanoparticles and second NIR window (1000–1700 nm) nanoprobes to realize precision bioimaging of tumors. This strategy finds use in other nano‐to‐microscale contrast agents to improve bioimaging signal‐to‐noise ratio and reduce long‐term cytotoxicity.