1：Experimental Design and Method Selection:

The study designed an in situ encapsulation method to immobilize glucose oxidase (GOx) within an oxygen-sensitive luminescent Cu(I) triazolate framework (MAF-2) at room temperature in a water-ethanol mixed solvent. The method leveraged the porous structure and O2-sensitivity of MAF-2 to create a composite (GOx@MAF-2) for glucose detection based on luminescence quenching by O2 consumption during enzymatic catalysis.

2：Sample Selection and Data Sources:

GOx from Aspergillus niger was used as the enzyme. Human blood serum samples were analyzed for glucose detection. Control samples included physically mixed GOx/MAF-2 and free GOx for comparison.

3：List of Experimental Equipment and Materials:

Equipment included Bruker D8 ADVANCE X-ray powder diffractometer (PXRD), TA Q50 thermogravimetric analyzer (TGA), Hitachi SU8010 scanning electron microscope (SEM) with energy-dispersive X-ray spectroscopy (EDS), Zeiss LSM 710 confocal laser-scanning microscope, EliteSizer dynamic light scattering (DLS) instrument, Hitachi F-7000 spectrofluorophotometer, JPB-607A dissolved O2 meter, and FluorChem M for SDS-PAGE imaging. Materials included Hdetz ligand, Cu2O nanoparticles, ascorbic acid, sodium acetate, trypsin, RhB, and various sugars for selectivity tests.

4：Experimental Procedures and Operational Workflow:

Synthesis involved mixing Cu2O nanoparticles, Hdetz ligand, and GOx in water-ethanol solvent under N2 protection at 25°C for 30 min, followed by centrifugation and washing. Characterization included PXRD, TGA, SEM-EDS, confocal microscopy, DLS, and luminescence measurements. Glucose sensing was performed by adding glucose to GOx@MAF-2 suspension in sodium acetate buffer (pH 5.5) and monitoring luminescence intensity over time. Stability and selectivity tests involved thermal treatment, protease incubation, and interference assays.

5：5) and monitoring luminescence intensity over time. Stability and selectivity tests involved thermal treatment, protease incubation, and interference assays. Data Analysis Methods:

5. Data Analysis Methods: Luminescence data were analyzed using Stern-Volmer equation for O2 sensitivity, Michaelis-Menten kinetics for enzyme activity, and linear regression for glucose concentration calibration. Statistical analysis included calculation of detection limits, Michaelis constants, and relative standard deviations.