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.
[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.
Servais, Anne-Catherine ✱; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Rozet, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Chiap, Patrice ; Centre Hospitalier Universitaire de Liège - CHU > Pharmacologie clinique
Boulanger, Bruno ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Rudaz, Serge
Crommen, Jacques ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Fillet, Marianne ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
✱ These authors have contributed equally to this work.
Language :
English
Title :
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.
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