Novel tetra-2-(biphenyl-4-yl)-1,3-benzoxazol-carboxamide nickel(II) phthalocyanine (NiTBPBXCAPc) and rGO were confirmed using FT-IR, UV-vis, XRD, TGA and Raman spectra. The NiTBPBXCAPc and rGO nanocomposite has been developed to detect hydroquinone (HQN) and chloramphenicol (CPC). NiTBPBXCAPc has been examined using cyclic voltammetry (CV), linear sweep voltammetry (LSV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS) analysis. The simultaneous CV analysis of HQN and CPC demonstrated the ability of NiTBPBXCAPc@rGO/GCE to execute simultaneous redox reactions. The voltammetric and amperometric limit of detection for HQN and CPC was determined to be 4.5 and 3.5 nM respectively, with a sensitivity of 0.446 and 0.416 μA M-1 cm-2. The amperometric LOD was observed to be 5 and 4 nM with a sensitivity of 0.235 and 0.288 μA M-1 cm-2. Additionally, the NiTBPBXCAPc@rGO/GC electrode is also used for real sample analysis with outstanding recovery. The long-term storage stability, reusability, and real-world sample analysis of the NiTBPBXCAPc@rGO/GC electrode demonstrated its use in environmental analysis.