1：Experimental Design and Method Selection:

A one-pot hydrothermal method was used to synthesize NH2-MIL-53(Al) nanosensor for fluorescent detection of TCs. The method involves the reaction between -NH2/-COOH groups of the nanosensor and -CO-/-OH groups of TCs, leading to fluorescence quenching via synergistic effects of photoinduced electron transfer (PET) and inner filter effect (IFE).

2：Sample Selection and Data Sources:

Milk samples were purchased from a local pasture. TCs standards and interfering substances (antibiotics, ions, amino acids, saccharides) were obtained from commercial sources.

3：List of Experimental Equipment and Materials:

Equipment includes field emission scanning electron microscope (FESEM), X-ray diffractometer (XRD), FT-IR spectroscope, UV-vis spectrophotometer, fluorescence spectrophotometer, HPLC system. Materials include AlCl3·6H2O, NH2-BDC, urea, DMF, various TCs and interferents, phosphate buffer solutions.

4：Experimental Procedures and Operational Workflow:

Synthesis of NH2-MIL-53(Al) via hydrothermal reaction at 150°C for 5 hours. Characterization using SEM, XRD, FT-IR, XPS, UV-vis, and fluorescence spectroscopy. Fluorescence detection involved adding nanosensor and TCs to a cuvette, incubating for 30 seconds, and measuring fluorescence spectra. Milk sample preparation involved protein removal using trichloroacetic acid and chloroform, followed by filtration.

5：Data Analysis Methods:

Quenching efficiency calculated using Stern-Volmer equation. Limit of detection (LOD) estimated based on standard deviation and slope. Statistical analysis performed using Minitab software. HPLC used for validation.