MoS2 nanoflakes were prepared by exfoliating commercial MoS2 powders with the assistance of ultrasound and graphene foam was synthesized by chemical vapor deposition using nickel foam as the template. MoS2‐graphene hybrid nanosheets were developed through the combination of MoS2 nanoflakes and graphene nanosheets by ultrasonic dispersion. The hybrid nanosheets were sprayed onto the ITO coated glass, which acts as an electrode for the simultaneously electrochemical determination of levodopa and uric acid. The MoS2‐graphene hybrid nanosheets were characterized by scanning electron microscopy, X‐ray diffraction and Raman spectroscopy. The results show that the hybrid nanosheets are composed of MoS2 and graphene with a sheet‐like morphology. The sensitivity of the electrode for levodopa and uric acid is 0.36 μA μM−1 and 0.39 μA μM−1, respectively. The electrode also shows low limit of detection, good selectivity, reproducibility and stability. And it is potential for use in clinical research.