The present study aimed to develop FeNi 3 nanoalloy-modified glassy carbon electrode (FeNi 3 /GCE) to detect paracetamol and tramadol drugs individually and simultaneously. Differential pulse voltammetry (DPV), chronoamperometry (CA) and cyclic voltammetry (CV) were applied to analyze the electrochemical properties of these drugs. The obtained results indicated the facilitation of paracetamol and tramadol oxidation on the FeNi 3 /GCE surface. The DPV findings confirmed the codetection of paracetamol and tramadol within a linear working range between 0.1 and 900.0 μM, with a limit of detection (S/ N = 3) of 10.0 and 8.2 nM, respectively. Multiple strengths were found for the synthesized electrode, including simplicity, high stability, potent reproducibility and excellent regeneration via simple polishing. The practical application of FeNi 3 /GCE in serum and urine specimens and pharmaceutical preparations confirmed high selectivity and sensitivity of this electrode to detect both paracetamol and tramadol.