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A pretreated pencil graphite electrode (PPGE) as an electrochemical sensor was developed and applied to measure diclofenac sodium (DIC). The effects of both potentiostatic and potentiodynamic strategies in the electrochemical pretreatment and performance of the electrode were studied, and it was concluded that the former offers better analytical sensitivity for electroanalytical purposes. PPGE displayed good electrocatalytic activity in comparison to nonpretreated PGE (NPGE). Differential pulse voltammetry (DPV) was used to determine DIC. Therefore, a calibration graph was plotted between the variation of anodic peak currents and the DIC concentration, which was found to be linear in the range 0.23–12.95 μmol/L with the detection limit (S/N = 3) of 0.12 μmol/L. PPGE was utilized to determine DIC in real samples such as biological and pharmaceutical ones, and the good recovery values obtained demonstrated the high accuracy of the modified electrode. [ABSTRACT FROM AUTHOR]