As a specific biomarker, neuron-specific enolase (NSE) is an essential clinical indicator for diagnosing small cell lung cancer. In this paper, a sandwich-type electrochemical immunosensor was designed for the quantitative detection of NSE. AuPt nanoblock spherical nanoarchitectonics (AuPt NSNs), a bimetallic nanoparticle with a rugged morphology, were utilized as the substrate, which could enhance the electronic conduction and increase the immobilization capacity of the primary antibody (Ab). Moreover, through a simple hydrothermal method, Au/CuO@CeO was prepared as a spiny core-shell nanocube with cerium dioxide (CeO) and gold nanoparticles (Au NPs) loading. The combination of CuO, CuO, and CeO showed favorable catalytic activity toward hydrogen peroxide (HO). Furthermore, the deposition of Au NPs on the spiny surface structure enhanced the specific surface area and biocompatibility, thereby rendering it more effective for loading the second antibody (Ab). As the label material, the Au/CuO@CeO achieved signal amplification and sensitive detection with the immunosensor. Under optimal conditions, the designed immunosensor possessed a broad linear range of 50 fg mL to 100 ng mL and a limit of detection of 31.3 fg mL, along with satisfactory performance in sensitivity, selectivity, and stability.
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