▎ 摘　　要

The self-assembled three-dimensional graphene nanohybrids with in situ-formed Fe3O4 and Pd nanoparticles on it (3DRGO_Fe3O4-Pd) are first synthesized by the one-pot solvothermal method, which have intrinsic peroxidase-like and oxidase-like activity. The catalytic mechanism is analyzed by the electron spin resonance (ESR), fluorescence, and electrochemical methods. The mimic enzyme catalytic activity of 3DRGO_Fe3O4-Pd is much higher than those of monometallic loaded nanohybrids and their physical mixture, probably caused by synergistic effect between Pd and Fe3O4 nanoparticles. The 3DRGO_Fe3O4-Pd nanohybrids was reproducible, stable, and reusable. After 10 cycles, the catalytic activity was still higher than 90%, and the morphology and structure were basically unchanged. Based on its high peroxidase-like activity, especially the enhanced affinity toward H2O2, a new colorimetric detection method for reduced glutathione (GSH) and glucose has been designed using H2O2 as an intermediary, which provides a simple, sensitive, and selective way to detect urine glucose of diabetes with a wide linear range and low detection limit.