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A novel multilayer‐shaped CeO2 with obvious electrocatalytic activity was synthesized using a simple heat treatment method. The structure and morphology of the multilayer‐shaped CeO2 were characterized by X‐ray diffraction, scanning electron microscopy, and transmission electron microscopy. Clenbuterol, a kind of β‐agonist drugs, has recently become a serious issue to human body due to the illegal addition in the food additive for livestocks. The drug residue in the human body may cause muscular pain, cardiac palpitation, glaucoma, prostatitis, dizziness and and even death in old people. Therefore, the detection of clenbuterol (CLB) has a important significance. The as‐prepared CeO2 was found to have unique electrocatalytic oxidation activities towards clenbuterol (CLB). The electrochemical sensor was constructed by fixing stable nafion‐modified multilayer‐shaped CeO2 film on a glassy carbon electrode. Compared with the CeO2‐modified electrode and the nafion‐modified electrode, the nafion‐modified multilayer‐shaped CeO2 electrode showed better electrocatalytic performance for clenbuterol in HClO4 solution. There was a good linear relationship between the oxidation peak current and the concentration of CLB between 0.39∼2.79 μmol/L, and the detection limit was 0.08 μmol/L (R=0.99). The nafion‐modified multilayer‐shaped CeO2 electrode exhibited high stability and reproducibility.

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