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In past decades, nanoscale metal‐organic frameworks (NMOFs) have drawn more and more attention in multimodal imaging and targeting therapy of various malignant cancers. Here, we proposed to dope 111In into fluorescent In‐based NMOFs (In‐MIL‐68‐NH2), with an attempt to prepare a new nanomedicine with great anticancer potential. As a proof of concept, the obtained NMOF (In‐MIL‐68/PEG‐FA) with targeting motifs is able to act as a fluorescent probe to achieve Hela cell imaging. Moreover, the Auger electron emitter 111In built in corresponding radioactive NMOF (111In‐MIL‐68/PEG‐FA) can bring clear damage to cancer cells, leading to a high cell killing rate of 59.3 % within 48 h. In addition, the cell cycle presented a significant dose‐dependent G2/M inhibiting mode, which indicates that 111In‐MIL‐68/PEG‐FA has the ability to facilitate the cancer cells to enter apoptotic program. This work demonstrated the potential of 111In‐labelled NMOFs in specific killings of cancer cells, providing a new approach to develop nanomedicines with theranostic function.

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