The voltammetric behaviour of minocycline at a water/nitrobenzene interface has been studied by normal, semi-differential and semi-integral cyclic voltammetry. The semi-differential cyclic voltammetry can be used as a rapid, simple method for determination of the antibiotic minocycline in the range of 5–200 ug/ml and the relative standard deviation is within 3%. Drug samples were analyzed and satisfactory results were found as compared with US Pharmacopoeia method.