A simple, rapid and highly sensitive electrochemical sensing platform has been developed for the simultaneous determination of Camylofin (CAM) and Analgine (ANG). The electrochemical oxidation based on bare and bulk zinc oxide nanoparticles (ZnO/NPs) and ionic liquid (IL) modified carbon paste electrode (ZnO/IL/MCPE) have been studied using cyclic voltammetry and square-wave voltammetric techniques. Under optimum conditions, the linearity range was from 1 mu mol L-1 to 100 mu mol L-1 and 0.2 mu mol L-1 to 100 mu mol L-1 for ANG and CAM, at bare and at ZnO/IL/MCPE, respectively in pH 7. The ZnO/IL/MCPE sensor was then explored toward the analysis of ANG and CAM in pharmaceutical formulation, real human serum and urine with excellent recoveries. The obtained results were compared successfully with respect to those obtained using the reported method. Moreover, this sensor is sensitive for the determination of ANG and CAM in the presence of common interference molecules uric acid (UA) and ascorbic acid (AA). The fabricated ZnO/IL/MCPE was demonstrated to exhibit a high sensitivity, good stability toward the sensing of ANG and CAM and was successfully used as a clinical assay and in quality assurance of pharmaceutical products. (C) 2019 The Electrochemical Society.