Atrazine (ATZ) represents an endocrine-disrupting pesticide posing significant threats to both the environment and human well-being. In this study, a novel turn-on electrochemical aptasensor was successfully developed for highly sensitive ATZ detection. It relied on Ni6MnO8@C/Au nanorods (Ni6MnO8@C/AuNR) and covalent-metal organic framework nanohybrids (MCA@Ce-MOF) with RecJf-catalyzed target recycling amplification. Notably, this marks the first instance of utilizing this strategy for ATZ detection. The substrate material, ultrathin Ni6MnO8@C/AuNR nanosheets, enhanced the specific surface area, conductivity, and biocompatibility, thereby facilitating biomolecule attachment and improving sensitivity. The scaffolds, hierarchically porous MCA@Ce-MOF, not only elevated the loading efficiency and surface concentration of signal molecules, but also strengthened the binding firmness of biomolecules. RecJf-catalyzed target recycling was triggered in the presence of ATZ, further magnifying electrochemical signals. Leveraging these unique attributes, the developed aptasensor exhibited exceptional ATZ detection performance with a low detection limit of 4.9 fg·mL−1, a wide linear range of 4 × 10−5–4 ng·mL−1, and a satisfactory recovery of 93.3–99.6% in corn samples. With its diverse signal amplification capabilities, this aptasensor holds promise for detecting various analytes in environmental monitoring applications.
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