A new POM-based hybrid, [δ-H 4 PMo V Mo 11 O 40 ](L) 5 •5H 2 O (1) (L = 4-methylpyridine-4-yl-1,8-naphthalene dicarboxylamide), was synthesized under hydrothermal conditions and characterized by IR spectroscopy, powder X-ray diffraction (PXRD), and X-ray photoelectron spectroscopy (XPS). 1 can acts as multifunctional uorescent sensor to detect metal cation (Fe 3+ ), anions (Cr 2 O 7 2− and CrO 4 2− ), and antibiotics (NFT = nitrofurantoin, NIT = nitrofurazone, OXY = oxytetracycline) in aqueous environment. The detection limits of 1 were 8.9 × 10 − 5 , 2.1 × 10 − 4 , 2.2 × 10 − 4 , 1.4 × 10 − 4 , 6.9 × 10 − 4 , and 6.1 × 10 − 4 mol•L − 1 for Fe 3+ , Cr 2 O 7 2− , CrO 4 2− , NIT, NFT, and OXY, respectively. Furthermore, the quenching mechanism between 1 and the different analytes can be regarded as energy competitive absorption.