This work outlines the scientific data concentrating on the determination of various antibiotics in medical drugs and substances by different physicochemical methods. The electrochemical behavior of widely used antibiotics such as streptomycin, tetracycline, and azithromicyn dihydrate from the macrolide group was studied for the purpose of selecting the determination conditions in pharmaceutical preparations by voltammetric methods. The voltammetric techniques for quantitative determination of streptomycin, tetracycline, and azithromicyn in different pharmaceutical preparations were developed and validated.