Determination of the purity of phenoxymethylpenicillin by micellar electrokinetic chromatography and reversed phase liquid chromatography on a monolithic silica column A micellar electrokinetic chromatographic and a fast reversed-phase liquid chromatographic method have been developed for determination of the purity of phenoxymethylpenicillin. The optimized running buffer composition was 40 mM phosphateborate -125 mM SDS -3.5% (v/v) methanol. The HPLC method employed a monolithic silica C18 column and a mobile phase composed of phosphate buffer, pH 3.5, and ACN, the flow-rate being 3.5 mL/min. Both methods were successfully validated. Linearity, intermediate precision, limits of quantitation, accuracy, and a good correlation of the HPLC and MEKC results were demonstrated. Both methods proved to be fast and reliable and sufficiently sensitive. A combination of the two methods can be very useful in impurity profiling.