NiFe2O4 nanoparticles (NPs) were employed to develop a novel electrochemical sensor having the detection limit up to nano mole with remarkable sensitivity. The modified electrochemical sensor was used with high efficacy in the detection of paracetamol (PCM) and dopamine (DA). The NPs being synthesized by combusting nickel acetate and ferric nitrate in the presence of sugar and monoethanolamine. The size, form, and morphology of the NPs were characterized using some advanced analytical techniques including energy-dispersive X-ray spectroscopy (EDS), field emission scanning electron microscopy (FESEM), and X-ray diffraction pattern (XRD). On the basis of characterizations, it was observed that the synthesized NPs exhibited a cubic crystal lattice having the size ranging from 10 to 12 nm as calculated by Debye-Scherrer equation. Next, the composite material, enhanced with graphite powder (GP), functioned as an electrode (NiFe2O4/GP) for the concurrent identification of PCM and DA through the utilization of cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methodologies. The results obtained from CV and DPV experiments at the surface of NiFe2O4/GP electrode reveals that the proposed electrochemical sensor having the remarkable sensitivity, achieving detection limits as low as 300.0 nM for DA and 400.0 nM for PCM, surpassing the values documented in previous research. The electrode demonstrated a linear range of 3.0–160.0 μM for PCM and 5.0–200.0 μM for DA. The oxidation peaks of DA and PCM were easily identifiable when differential pulse voltammetry and cyclic voltammetry were conducted with scan rates of 100 mVs−1 and 50 mVs−1, respectively. The measurements were performed in a phosphate buffer solution with a pH of 6.0. The electrodes yielded positive results when applied to actual samples of PCM and DA.