title: Evaluation of an International Pharmacopoeia method for the analysis of saquinavir (mesilate) bulk drugs by liquid chromatography.
abstract: A single gradient LC method for the determination of related substances in both saquinavir (SQV), saquinavir mesilate (SQVM) has been published in a consultation document of the International Pharmacopoeia, WHO Drug Information. The method uses a base deactivated reversed phase C18 column (25 cm x 4.6 mm i.d.), 5 microm kept at a temperature of 30 degrees C. The mobile phases consist of acetonitrile, methanol, phosphate buffer pH 3.4 and water. The flow rate is 1.0 ml/min. UV detection is performed at 220 nm. A system suitability test (SST) is described to govern the quality of the separation. The separation towards SQV(M) components was investigated on 18 C18 columns and correlation was made with the column classification system developed in our laboratory. The method was evaluated using a Hypersil BDS C18 column (25 cm x 4.6 mm i.d.), 5 microm. A central composite design was applied to examine the robustness of the method. The method shows good precision, linearity, sensitivity and robustness. SQV(M) commercial samples of bulk drugs were examined using this method.
authors.affiliation: Laboratorium voor Farmaceutische Analyse, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, Leuven, Belgium.
authors.forename: Raja
authors.initials: R
authors.lastname: Yekkala
authors.forename: Lena
authors.initials: L
authors.lastname: Vandenbosch
authors.forename: Jos
authors.initials: J
authors.lastname: Hoogmartens
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D000465:Algorithms; D019380:Anti-HIV Agents / Q000032:analysis*; D002853:Chromatography, Liquid; D007202:Indicators and Reagents; D010602:Pharmacopoeias as Topic; D012015:Reference Standards; D012044:Regression Analysis; D015203:Reproducibility of Results; D019258:Saquinavir / Q000032:analysis*; D012996:Solutions
chemical_list: D019380:Anti-HIV Agents; D007202:Indicators and Reagents; D012996:Solutions; D019258:Saquinavir