In this study, a highly sensitive, selective and cost‐effective electrochemical nano‐sensor has been developed for the first time so as to facilitate the simultaneous and low‐level detection of acetaminophen (paracetamol, PAR), ascorbic acid (A) and acetylsalicylic acid (ASA) ternary mixture. The sensor is based on nano‐sepiolite clay (SEP) with multiwall carbon nanotubes (MWCNTs) onto electrochemically pretreated pencil graphite electrode (pPGE). The surface properties of the sensor were examined by using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM) techniques. The pH effect, composition of modifiers, immobilization time, deposition potential and deposition time values were optimized to reach the best response of PAR, A and ASA. Moreover, in optimum analytical conditions, adsorptive stripping differential pulse voltammmetric (AdsDPV) method was developed for the simultaneous analysis of the ternary mixtures concerned by using SEP/MWCNTs/pPGE sensor. This sensor exhibited the low detection limits of 0.018, 0.042 and 0.047 μM for PAR, A and ASA ternary mixture, respectively. The developed AdsDPV method was applied for quantitative determination of PAR, A and ASA in the pharmaceutical formulation. The recovery experiments were carried out to control the accuracy and precision of the method. The obtained voltammetric recoveries were comparable with the HPLC data given in the literature.

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