The synthesis of NiO/NiCo2O4 nanoparticles by an eco‐friendly, fast, simple and cost‐effective approach employing Urtica extract is reported in this study. The NiO/NiCo2O4 nanocomposite were characterized using VSM, FTIR, XRD, and SEM techniques. Moreover, to construct a modified carbon paste electrode, NiO/NiCo2O4 were employed and this sensor was used for dopamine (DA) detection. Using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques, the electrochemical behavior of dopamine at the NiO/NiCo2O4/CPE was investigated. Analysis of dopamine, with a limit of detection (LOD) equal to 0.04 μM, in the concentration range of 0.1–100.0 μM, was facilitated by NiO/NiCo2O4/CPE. Moreover, the satisfactory selectivity for DA determination in the presence of uric acid (UA) and ascorbic acid (AA), was obtained. The suggested new sensor displayed a good reproducibility, sensitivity, and stability for determination of DA in drug and biological samples.