The spherical Au nanoparticles/3D flower-like graphene was prepared by a facile and low-cost electrochemical method and used for sensitive determination of nitrite. Display omitted In this paper, the spherical Au nanoparticles and 3D flower-like structure graphene were successively deposited on glassy carbon electrode (GCE) (Au/f-GE/GCE) via a facile and two-step electrodeposition method for the detection of nitrite ions (NaNO2). The morphology and composition elements were confirmed by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction measurements (XRD). Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to evaluate the electrochemical behaviors of NaNO2 on the as-prepared electrode. Compared to f-GE/GCE and Au/GCE, Au/f-GE/GCE showed a sharp and obvious oxidation peak at 0.78V. The oxidation peak current of NaNO2 was linearly proportional to its concentration in the range from 0.125 to 20375.98μM, with a detection limit of 0.01μM (at S/N=3). Furthermore, the experiment results also showed that the as-prepared electrode exhibited excellent reproducibility and long-term stability, as well as good recovery when applied to the determination of NaNO2 in pickled pork samples.