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Express determination of antibiotics is an extremely important task today. Portable electrochemical microdevices are a viable alternative to traditional methods of analysis. The development of such devices requires the study of redox processes in detail. This article is devoted to the comparative study of the electrochemical behavior of chloramphenicol in water solvents in standard laboratory and portable microelectrochemical cells. It was found that the electrochemical reduction of chloramphenicol proceeds via a 3-electron mechanism to the formation of a dimer. In the transition from the macrocell to the microcell, a decrease in the electrochemical reduction current and a shift of the peak potential to the cathode region are observed, which is apparently associated mainly with the type of the electrode material. The best characteristics of the direct electrochemical response were obtained in the differential pulse voltammetry mode. Under the selected operating parameters, the peak current of the electrochemical reduction of chloramphenicol is linearly dependent on the concentration of the antibiotic in the range of 2∙10–3–1∙10–5 M with a detection limit of 3∙10–5 M. Obtained characteristics are sufficient for the quality control of pharmaceuticals and can be improved through the use of organic and hybrid modifiers of the working electrode surface.