| Summary: | Two-dimensional (2D) MXenes have shown a great potential for chemical sensing due to their electric properties. In this work, a Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub>/polypyrrole (MXene/PPy) nanocomposite has been synthesized and immobilized into a glassy carbon electrode to enable the simultaneous recognition of dopamine (DA) and uric acid (UA) under the interference of ascorbic acid (AA). The multilayer Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> MXene was prepared via the aqueous acid etching method and delaminated to a single layer nanosheet, benefiting the in-situ growth of PPy nanowires. The controllable preparation strategy and the compounding of PPy material remain great challenges for further practical application. A facile chemical oxidation method was proposed to regulate magnitude and density during the forming process of PPy nanowire, which promotes the conductivity and the electrochemical active site of this as-prepared nanomaterial. The MXene/PPy nanocomposite-modified electrode exhibited the selective determination of DA and UA in the presence of a high concentration of AA, as well as a wide linear range (DA: 12.5–125 μM, UA: 50–500 μM) and a low detection limit (DA: 0.37 μM, UA: 0.15 μM). More importantly, the simultaneous sensing for the co-existence of DA and UA was successfully achieved via the as-prepared sensor.
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