Ensuring food safety necessitates the reliable detection of biogenic amines (BAs) such as tyramine, which serve as key indicators of food spoilage and potential food poisoning. In this study, we report the rational design and synthesis of a three‐dimensional luminescent MOF (LMOF), Zn(II)‐MOF, Zn(TA) 2 (BP) 2 n , constructed from Zn(II), terephthalic acid (TA), and 4,4′‐bipyridine (4,4‘‐BP). This MOF exhibits strong fluorescence and functions as a highly selective “turn‐on” sensor for tyramine in aqueous solutions, achieving a low detection limit of 13 µM (1.78 ppm, R 2 = 0.993). The observed selective fluorescence enhancement is attributed to specific host–guest interactions and regulated electron transfer pathways, as supported by density functional theory (DFT) calculations. Importantly, the robust MOF maintains its structural integrity and sensing performance when applied to real food matrices, including fish‐meat and milk, demonstrating practical utility in complex sample environments. Given the limited availability of MOF‐based sensors capable of selectively detecting tyramine over other BAs in both aqueous and food systems, this work represents a significant advancement in the field. Therefore, this establishes a clear structure–performance relationship and highlights the potential of luminescent Zn(II)‐BPTA‐MOF as a reliable, practical, and effective tool for tyramine monitoring, contributing meaningfully to food quality assurance and public health protection.
Sarkar et al. (Sun,) studied this question.