Abstract A unique luminescent lanthanide metal–organic framework (LnMOF)–based fluorescence detection platform was utilized to achieve sensitive detection of vomitoxin (VT) and oxytetracycline hydrochloride (OTC‐HCL) without the use of antibodies or biomolecular modifications. The sensor had a fluorescence quenching constant of 9.74 × 10 6 M −1 and a low detection limit of 0.68 nM for vomitoxin. Notably, this is the first example of a Tb‐MOF sensor for fluorescence detection of vomitoxin. We further investigated its response to two mycotoxins, aflatoxin B1 and ochratoxin A, and found that their Stern–Volmer fluorescence quenching constants were lower than those of VT. In addition, the fluorescence sensor realized sensitive detection of OTC‐HCL with a detection limit of 0.039 μM. In conclusion, the method has great potential as a sensitive and simple technique to detect VT and OTC‐HCL in water.