title: Development of a liquid chromatography method for the analysis of josamycin.
abstract: Out of three methods for the analysis of josamycin, the best one was selected and used as starting point for further development. A central composite design was applied to find the most influencing parameters and to optimize the chromatographic conditions and a full factorial design was used to perform a robustness study. The final method uses a Hypersil ODS column 5microm, 250mmx4.6mm i.d. maintained at 45 degrees C. The mobile phase is composed of acetonitrile-phosphate buffer (pH 3, 0.2moll(-1))-tetrabutylammonium hydrogen sulphate 0.2moll(-1)-water (21:5:3:71, v/v/v/v). Strongly retained impurities after the main peak require gradient elution, which is obtained by increasing linearly the acetonitrile concentration (from 21% to 50%, v/v) and decreasing the TBA concentration (from 3% to 0%, v/v) in the mobile phase. The total run time was 65min. UV detection is performed at 232nm and the flow rate is 1ml/min. The method shows good selectivity, precision, linearity and sensitivity. Five commercial bulk samples were analyzed.
authors.affiliation: Laboratory for Pharmaceutical Analysis, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, O&N 2, Herestraat 49 (PB 923), B-3000 Leuven, Belgium.
authors.forename: F
authors.initials: F
authors.lastname: Daidone
authors.forename: R
authors.initials: R
authors.lastname: Heuvelmans
authors.forename: L
authors.initials: L
authors.lastname: Aerden
authors.forename: J
authors.initials: J
authors.lastname: Hoogmartens
authors.forename: E
authors.initials: E
authors.lastname: Adams
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D015570:Josamycin / Q000032:analysis*; D012680:Sensitivity and Specificity
chemical_list: D015570:Josamycin