ABSTRACT One 3D Zn‐MOF , namely, {[Zn 2 (L)(OH)(DMF)]} n was selected based on the flexible ether oxygen carboxylic acid 3‐(3,5‐dicarboxylatobenzyloxy)benzoic acid (H 3 L). Zn‐MOF was able to specifically recognize the biomarker methylmalonic acid (MMA) and antibiotic tetracycline (TC) through fluorescence enhancement and ratio mechanism, with the detection limits (LOD) as low as 1.29 and 0.26 μM, respectively. It also has high selectivity and rapid response characteristics. In particular, the visual detection was significantly enhanced in the presence of Tb 3+ through antenna effect. To explore the potential application, fluorescent test strips and mixed matrix membrane (MMM) were successfully prepared to realize visual detection. The recovery rates of MMA and TC in simulated urine and actual water systems were 95.3%–100.5% and 93.5%–94.7%, respectively, indicating that Zn‐MOF provided the possibility for detecting biomarker and antibiotic in practical systems.