<p>The electrochemical properties of the antiarrhythmic drug amiodarone were investigated using square-wave and cyclic voltammetry techniques in Britton–Robinson buffer solution (pH 5.0) with a disposable electrochemical-activated pencil graphite electrode. In cyclic voltammetry measurements, it was observed that amiodarone exhibited a well-defined irreversible oxidation peak at a voltage of approximately + 0.94 V. With optimized instrument parameters, amiodarone exhibited a linear response in the concentration range of 0.125 to 6.862 µg/mL in Britton–Robinson buffer solution (pH 5.0) on a disposable electrochemical-activated pencil graphite electrode. The resulting calibration curve was Ip (µA) = 0.113 <i>C</i> (µg/mL) + 0.039 (<i>r</i> = 0.998, <i>n</i> = 9). The limit of detection and limit of quantification values for the voltammetric method were determined to be 0.027 µg/mL and 0.089 µg/mL, respectively. The simplicity, rapidity, and sensitivity of the developed voltammetric method are considered to be important advantages. In addition, the applicability of the proposed voltammetric method to drug and urine samples demonstrated the selectivity of the method. The results of the voltammetric technique developed for the analysis of amiodarone in pharmaceutical samples were supported by spectrophotometric results.</p> Graphical Abstract <p></p>