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In this paper, ultrathin graphene (GN) nanosheets were uniformly decorated with nickel (Ni) nanoparticles, as confirmed by scanning electron microscopy and transmission electron microscopy. This GNNi hybrid exhibited excellent accumulation and catalytic capacity for the simultaneous detection of sunset yellow and tartrazine, two colorants commonly found mixed in foodstuffs. The electrochemical reaction mechanism of sunset yellow and tartrazine were studied in detail on the GNNi nanocomposite modified glassy carbon electrode. In square wave voltammetry measurements, the oxidation peak potentials of sunset yellow and tartrazine were separated by about 250 mV. This novel proposed voltammetric method has good selectivity which was successfully applied for the simultaneous determination of sunset yellow and tartrazine in some food sample extracts. [ABSTRACT FROM AUTHOR]