Reference : Nonaqueous capillary electrophoresis method for the enantiomeric purity determination...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/9010
Nonaqueous capillary electrophoresis method for the enantiomeric purity determination of S-timolol using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin: validation using the accuracy profile strategy and estimation of uncertainty.
English
Marini Djang'Eing'A, Roland mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Servais, Anne-Catherine mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Rozet, Eric mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Chiap, Patrice [Centre Hospitalier Universitaire de Liège - CHU > > Pharmacologie clinique >]
Boulanger, Bruno [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Rudaz, Serge [> > > >]
Crommen, Jacques mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Hubert, Philippe mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Fillet, Marianne mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
2006
Journal of Chromatography. A
Elsevier Science
1120
1-2
102-11
Yes (verified by ORBi)
International
0021-9673
Amsterdam
The Netherlands
[en] Antihypertensive Agents/chemistry/isolation & purification ; Electrophoresis, Capillary/methods ; Molecular Structure ; Reference Standards ; Regression Analysis ; Reproducibility of Results ; Stereoisomerism ; Timolol/chemistry/isolation & purification ; beta-Cyclodextrins/chemistry/standards
[en] Nonaqueous capillary electrophoresis (NACE) was successfully applied to the enantiomeric purity determination of S-timolol maleate using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD) as chiral selector. With a background electrolyte made up of a methanolic solution of 0.75 M formic acid, 30 mM potassium camphorsulfonate and containing 30 mM HDMS-beta-CD, the determination of 0.1% of R-timolol in S-timolol could be performed with an enantiomeric resolution of 8.5. Pyridoxine was selected as internal standard. The NACE method was then fully validated by applying a novel strategy using accuracy profiles. It is based on beta-expectation tolerance intervals for the total measurement error which includes trueness and intermediate precision. The uncertainty of measurements derived from beta-expectation tolerance intervals was estimated at each concentration level of the validation standards. To confirm the suitability of the developed and validated method, several real samples of S-timolol maleate containing R-timolol maleate at different concentrations were analysed and the results were compared to those obtained by liquid chromatography.
http://hdl.handle.net/2268/9010
10.1016/j.chroma.2006.03.104

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