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Carbon nitride and WS 2 nanocomposite (CN-WS 2 ) with excellent photoelectric activity was prepared by one-step thermal polymerization. By the new strategy of simultaneously loading C and N elements on pure WS 2 , the formation of CN-WS 2 brings high mobility, ultra-fast charge carrier separation and transport, and slows down the recombination rate of electrons and holes. Then, a novel photoelectrochemical biosensor was constructed for 5-formylcytosine detection based on CN-WS 2 composite, aldehyde reaction probe (ARP) and ZnFe 2 O 4 , where CN-WS 2 composite was employed as photoactive material, ARP was used as 5-formylcytosine capture reagent, and ZnFe 2 O 4 was adopted as artificial mimic enzyme. Under the catalysis effect of ZnFe 2 O 4 , 4-chloro-1-naphthol was quickly oxidized by H 2 O 2 to produce the insoluble substance of benzo-4-chlorohexadienone, which would be deposited on the electrode surface and caused a decreased PEC response. Under optimal experimental conditions, the biosensor showed low detection limit of 3 pM. This method can also discriminate 5-formylcytosine with other cytosine derivatives. More importantly, the applicability of this method was demonstrated by assessing the effect of antibiotics on the content of 5-formylcytosine in the root, stem and leave of maize seedlings., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2019 Elsevier B.V. All rights reserved.)