title: Improved liquid chromatographic method with pulsed electrochemical detection for the analysis of gentamicin.
abstract: The official method for the determination of the composition and related substances of gentamicin prescribed by the European Pharmacopoeia (Ph. Eur.) is liquid chromatography combined with pulsed electrochemical detection (LC-PED). However, this method utilizes a polymer stationary phase which shows rather low efficiency towards the separation of the main gentamicin components. Moreover, the mobile phase contains a lot of non volatile salts: sodium sulphate and sodium octanesulphonate. Following a comparative study, the most performant LC-PED method has been evaluated and validated using a reversed phase C18 column (C18, 250 x 4.6mm ID, 110 A, 5 microm) kept at 35 degrees C with a mobile phase containing volatile ion pairing agents: trifluoroacetic acetic acid (TFA) and pentafluoropropionic acid (PFPA). In addition to the selectivity of the main gentamicin components and its related substances, the method is repeatable, linear and proves to be robust. It is also applicable to a wider number of C18 columns.
authors.affiliation: Laboratorium voor Farmaceutische Analyse, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, O&N2, PB 923, Herestraat 49, B-3000 Leuven, Belgium.
authors.forename: Vicky
authors.initials: V
authors.lastname: Manyanga
authors.forename: Katjusa
authors.initials: K
authors.lastname: Kreft
authors.forename: Blaz
authors.initials: B
authors.lastname: Divjak
authors.forename: Jos
authors.initials: J
authors.lastname: Hoogmartens
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004563:Electrochemistry / Q000379:methods*; D005466:Fluorocarbons / Q000737:chemistry; D005839:Gentamicins / Q000032:analysis* / Q000737:chemistry; D006595:Hexosamines / Q000032:analysis / Q000737:chemistry; D012853:Sisomicin / Q000032:analysis / Q000737:chemistry; D014269:Trifluoroacetic Acid / Q000737:chemistry
chemical_list: D005466:Fluorocarbons; D005839:Gentamicins; D006595:Hexosamines; C033093:perfluoropropionic acid; D014269:Trifluoroacetic Acid; C007265:2-deoxystreptamine; D012853:Sisomicin