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To explore a novel colorimetric biosensor with high sensibility and selectivity, a new Wells–Dawson-type polyoxometalate (POM)-based metal–organic framework (MOF) with an eightfold helix, [Cu9(FKZ)12(H2O)8][H3P2W18O62]2·4H2O (CuFKZP2W18) (HFKZ = 1-(2,4-difluorophenyl)-1,1-bis[(1H-1,2,4-triazol-1-yl)methyl] ethanol), was successfully synthesized; then, polypyrrole (PPy) was introduced to fabricate CuFKZP2W18/PPy(n) nanocomposites (n = 7%, 15%, 30%) via a facile in situ oxidation polymerization process. All the results indicate that CuFKZP2W18/PPy(15%) as a colorimetric biosensor exhibits lower limits of detection (0.07 μM towards H2O2 and 0.627 μM towards ascorbic acid), smaller Km values (0.106 mM for H2O2 and 0.042 mM for o-phenylenediamine) and higher sensitivity (0.0227 1 μM−1 towards H2O2 and 0.0025 1 μM−1 to ascorbic acid) than most reported enzyme mimetics to the best of our knowledge. [ABSTRACT FROM AUTHOR]