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

Marini, RD;Servais, AC;Rozet, E.;Chiap, P.;Fillet, M;et.al.
(2006) 29th International Symposium on High Performance Liquid Separations and Related Techniques (HPLC 2005) — Location: Stockholm(Sweden) (26.June.2005)

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Authors
  • Marini, RD
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  • Servais, AC
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  • Rozet, E.
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  • Chiap, P.
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  • Fillet, M
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Abstract
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-P-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 P-expectation tolerance intervals for the total measurement error which includes trueness and intermediate precision. The uncertainty of measurements derived from P-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. (c) 2006 Elsevier B.V. All rights reserved.
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Marini, R., Servais, A., Rozet, E., Chiap, P., Boulanger, B., Rudaz, S., Crommen, J., Hubert, P., & Fillet, M. (2006). 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. Journal of Chromatography A, 1120(1-2), 102-111. https://doi.org/10.1016/j.chroma.2006.03.104 (Original work published 2006)