AbstractTo fulfill the emerging demand for drug therapy, the Y/Tb/Gd ternary layered rare‐earth hydroxide nanocone is developed as a new multifunctional delivery system for one of the most popular drugs, aspirin. Dodecyl sulfate intercalation is firstly used for the drug carrier which can form hollow nanocones and owns low binding energy, leading to the facile synthesis of organic–inorganic hybrid drug delivery system. The aspirin can be loaded rapidly (as short as 5 min) and released continuously (as long as 48 h) by YTG system through anion exchange, which will be favorable for sustained therapy. Meanwhile, the intercalated aspirin can enhance the green light luminescence of Tb3+ with peak position at 543 nm through energy transfer, which can be utilized as fluorescence probe to monitor the drug loading and release process. The magnetization of Gd3+ can also be improved by structural evolution induced by aspirin intercalation, which can be applied as magnetic resonance imaging contrast agent simultaneously. The current research provides a novel pathway for the invention of multifunctional drug delivery system, which hopefully is to be put into service in biomedical fields in the near future.
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