A fluorescent method for detection of tetracyclines (TCs) in milk was developed by using the NH 2 -MIL-53(Al) nanosensor synthesized via a one-pot hydrothermal method. The nanosensor had a crystalline nanoplates structure with rich groups of −NH 2 and −COOH. The −NH 2 /−COOH of NH 2 -MIL-53(Al) reacted with the −CO−/−OH of TCs to form a complex. The electron of −NH 2 /−COOH from the NH 2 -BDC ligand transferred to the −CO−/−OH of TCs. −NH 2 of the NH 2 -MIL-53(Al) interacted with the −CO−/−OH of TCs by hydrogen bonding. The quenching efficiency of the inner filter effect (IFE) was calculated to contribute 57−89%. The synergistic effect of photoinduced electron transfer (PET) and IFE account for fluorescence quenching. TCs were quantitatively detected in milk samples with recoveries of 85.15−112.13%; the results were in great accordance with high-performance liquid chromatography (HPLC) (P > 0.05), confirming the NH 2 -MIL-53(Al) nanosensor has potential applicability for the detection of TCs in food matrix.

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