AbstractIn this study, a novel strategy to amplify electrochemical signals by mesoporous PdPt nanoparticles with core‐shell structures anchored on a three‐dimensional PANI@CNTs network as nanozyme labels (PdPt/PANI@CNTs) was proposed for the sensitive monitoring of α‐fetoprotein (AFP, Ag). First, the mesoporous PdPt nanoparticles prepared by a facile chemical reduction method had excellent biocompatibility with biomolecules, which could capture a large amount of AFP‐Ab2 (Ab2) and exhibit plentiful pores to entrap more thionine (Thi) into mesoporous PdPt nanoparticles with enhanced loading and abundant active sites. Furthermore, the resulting mesoporous PdPt nanoparticles were abundantly dotted on the surface of a three‐dimensional PANI@CNTs network with excellent conductivity and a high specific surface area through the bonding of the amino group to form PdPt/PANI@CNTs nanozyme labels. Most importantly, the as‐prepared PdPt/PANI@CNTs nanozyme labels exhibited unexpected enzyme‐like activity towards the reduction of hydrogen peroxide owing to the highly indexed facets, enhancing the current response to realize signal amplification. In view of the advantages of nanozyme labels and the involvement of gold nanoparticles (AuNPs, which behave as electrode materials) for the sensitive determination of AFP, the as‐developed immunosensor could obtain a dynamic working range of 0.001 ng mL−1–100.0 ng mL−1 at a detection limit of 0.33 pg mL−1 via DPV (at 3σ). Furthermore, the nanozyme‐based electrochemical immunosensor exhibited remarkable analytical performance, which brought about feasible ideas for disease diagnosis in the future.
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