In this paper, a highly effective electrochemical sensor based on graphene (Gr)/copper phthalocyanine (CuPc) nanocomposites was successfully designed and achieved. The morphology of Gr/CuPc nanocomposites was characterized by UV-vis, IR, Raman spectra and scanning electron microscopy (SEM). Gr/CuPc nanocomposites were gathered on the surface of the glassy carbon electrode (GCE), and the performence of Gr/CuPc/GCE toward chloramphenicol (CAP) and florfenicol (FF) was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The Gr/CuPc/GCE presented good electrochemical properties, stability, reproducibility, excellent anti-interference ability and satisfying recovery rate in real samples for the detection of CAP and FF. The performance of Gr/CuPc/GCE exhibited a linear ranging from 1.0 × 10 −7 to 2.0 × 10 −5 M with a detection limit of 2.7 × 10 −8 M (−0.652 V vs. Hg/Hg 2 Cl 2 , S/N = 3) toward CAP. For FF, it exhibited a linear ranging from 1.0 × 10 −6 to 3.0 × 10 −5 M with a detection limit of 7.5 × 10 −7 M (−0.863 V vs. Hg/Hg 2 Cl 2 , S/N = 3). Furthermore, it is for the first time that FF is determined by electrochemical sensor through nanocomposites modified electrode. This proposed electrochemical sensor can provide an opportunity for convenient and reliable determination of CAP or FF.

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