| Summary: | Two triple interpenetrating Zn(II)-based MOFs were studied in this paper. Named [Zn<sub>6</sub>(1,4-bpeb)<sub>4</sub>(IPA)<sub>6</sub>(H<sub>2</sub>O)]<sub>n</sub> (<b>MOF-1</b>) and {[Zn<sub>3</sub>(1,4-bpeb)<sub>1.5</sub>(DDBA)<sub>3</sub>]<sub>n</sub>·2DMF} (<b>MOF-2</b>), {1,4-bpeb = 1,4-bis [2-(4-pyridy1) ethenyl]benze, IPA = Isophthalic acid, DDBA = 3,3′-Azodibenzoic acid}, they were synthesized by the hydrothermal method and were characterized and stability tested. The results showed that <b>MOF-1</b> had good acid–base stability and solvent stability. Furthermore, <b>MOF-1</b> had excellent green fluorescence and with different phenomena in different solvents, which was almost completely quenched in acetone. Based on this phenomenon, an acetone sensing test was carried out, where the detection limit of acetone was calculated to be 0.00365% (volume ratio). Excitingly, the <b>MOF-1</b> could also be used as a proportional fluorescent probe to specifically detect tryptophan, with a calculated detection limit of 34.84 μM. Furthermore, the mechanism was explained through energy transfer and competitive absorption (fluorescence resonance energy transfer (FRET)) and internal filtration effect (IFE). For antibacterial purposes, the minimum inhibitory concentrations of <b>MOF-1</b> against <i>Escherichia coli</i> and <i>Staphylococcus aureus</i> were 19.52 µg/mL and 39.06 µg/mL, respectively, and the minimum inhibitory concentrations of <b>MOF-2</b> against <i>Escherichia coli</i> and <i>Staphylococcus aureus</i> were 68.36 µg/mL and 136.72 µg/mL, respectively.
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