The modification of traditional electrodes with mesoporous carbons is a promising strategy to produce high performance electrodes for electrochemical sensing. The high surface area of mesoporous carbons provides a large number of electroactive sites for binding analytes. Controlling the pore size and structure of mesoporous carbons and modifying their electronic properties via doping offers additional benefits like maximizing transport and tuning the electrochemical processes associated with analyte detection. This work reports a facile method to produce sulfur-doped ordered mesoporous carbon materials (S-OMC) with uniform pore structure, large pore volume, high surface area and semigraphitic structure. The synthesis used thiophenol as a single source of carbon and sulfur, and iron as a catalyst for low temperature carbonization. The S-OMC material was deposited on a glassy carbon electrode and used as a sensor with high sensitivity (11.7 A L mol−1) and selectivity for chloramphenicol detection in presence of other antibiotics. As a proof-of-concept, the sensor was applied to the direct analysis of the drug in reconstituted powdered milk and in commercial eye drops.