Chloramphenicol (CAP) is a widely used, broad spectrum antibiotic that contains a nitrobenzene moiety with a possible poisonous feature. Thus, the development of low cost, simple, and rapid analytical methods for the reliable CAP quantification is necessary. Starting from the nitro group electroactivity, the cyclic voltammetric properties of CAP were investigated at the common commercially available, disposable pencil graphite electrode (PGE). The effect of the electrode material, the electrolyte pH and the potential scan rate were investigated. At 2H type PGE, the CAP cyclic voltammograms presented an anodic and two cathodic diffusion controlled, pH-dependent peaks, each involving the exchange of two electrons and two protons. Based on CAP main reduction peak at PGE in pH 5.00 Britton Robinson buffer, a square wave voltammetric (SWV) method was developed for its quantification from 2.50 × 10−6 to 7.50 × 10−4 mol L−1 with a limit of detection (LoD) of 1.39 × 10−6 mol L−1. Moreover, the anodic peak was also employed for the first time for a CAP linear sweep voltammetric (LSV) assay (2.50 × 10−6 to 1.00 × 10−3 mol L−1; LoD 6.09 × 10−7 mol L−1 CAP). Both voltammetric methods using the cost-effective PGE were applied for the determination of CAP in pharmaceuticals, obtaining recoveries of 100.9 ± 1.4% (relative standard deviation of 3.54%) for SWV and 100.7 ± 1.4% (relative standard deviation of 3.55%) for LSV. [ABSTRACT FROM AUTHOR]