The analysis of amikacin by liquid chromatography using a column packed with poly(styrene-divinylbenzene) and pulsed electrochemical detection on a gold electrode is described. A two-step gradient was necessary to obtain a good separation together with a reasonable analysis time of 60 min. The mobile phases consisted of an aqueous solution of 1 g/l or 60 g/l sodium sulfate, 1.8 g/l sodium octanesulfonate and 50 ml/l 0.2 M phosphate buffer, pH 3.0. Sodium hydroxide was added postcolumn. The influence of the different chromatographic parameters on the separation was investigated. When a number of commercial samples of amikacin was analyzed using this method, ten different components were separated.