SnO2‐CNF was prepared by coaxial blending technology, and MoS2 was grown uniformly on SnO2‐CNF composite by adding a hydrothermal post‐treatment step. The uniform distribution of MoS2 on one‐dimensional SnO2‐CNF can effectively establish a layered three‐dimensional structure. Accordingly, the prepared MoS2‐coated SnO2‐CNF composite material has higher surface area and more active sites to obtain better electrochemical performance. We constructed an electrochemical sensor within the composite material with enhanced performance to realize the simultaneous and highly sensitive detection of phenacetin and indomethacin. The sensor has linear ranges of 0.050–7200 μM and 0.05–500 μM, respectively, and the detection limits were 0.016 μM and 0.013 μM. Furthermore, the sensor has good anti‐interference ability and stability, which also achieves good recovery rate in the actual sample detection.
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