Defining a system suitability limit to decide on column deterioration and to facilitate column transfers in chiral super
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RESEARCH PAPER
Defining a system suitability limit to decide on column deterioration and to facilitate column transfers in chiral supercritical fluid chromatography Sven Declerck 1 & Yvan Vander Heyden 1 & Debby Mangelings 1 Received: 2 August 2019 / Revised: 17 September 2019 / Accepted: 24 September 2019 # Springer-Verlag GmbH Germany, part of Springer Nature 2019
Abstract The separation of enantiomers is an important requirement during the entire drug life cycle in the pharmaceutical industry. Highperformance liquid chromatography and supercritical fluid chromatography (SFC) are the main chromatographic techniques used to separate enantiomers. Since chiral stationary phases are often extensively used once a method has been developed, columns will age and must be replaced after a certain period. However, no practical guidelines exist to determine when a column is deteriorated or to decide whether a transfer to another column (with the same chiral selector) is successful. In this study, a system suitability limit for resolution was defined, based on an intermediate (time-different) precision study in SFC on four immobilized polysaccharide-based columns that only differed in manufacturer or particle size. This system suitability limit could be used to decide on column deterioration or as a requirement to evaluate whether a separation transfer was successful. Some method adaptations may be necessary to obtain successful transfers. An approach was proposed, which helped the analyst to make successful transfers. Keywords Supercritical fluid chromatography . Enantioseparations . Intermediate-precision study . System suitability . Transfer
Introduction Due to enantioselective recognition processes in the human body, one enantiomer of a pharmaceutical will interact preferentially with a drug receptor, resulting in the expected pharmacodynamic and pharmacokinetic responses. The other enantiomer of the drug will interact differently (not or less selective) with the receptor, but may interact (better) with another receptor, which will result in no, another, a lower or an unexpected pharmacological response [1, 2]. For example, thalidomide possesses an unstable chiral carbon atom that allows Published in the topical collection featuring Female Role Models in Analytical Chemistry. Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-019-02173-7) contains supplementary material, which is available to authorized users. * Debby Mangelings [email protected] 1
Department of Analytical Chemistry, Applied Chemometrics and Molecular Modelling (FABI), Vrije Universiteit Brussel (VUB), Laarbeeklaan 103, 1090 Brussels, Belgium
racemization and the occurrence of the two enantiomers in the body [3]. The administration of the R-enantiomer provides the desired pharmacologic response, i.e. treat morning sickness of pregnant women. The other enantiomer does not show the pharmacological response but is teratogenic. The marketed thalidomide drug was administered as a racemic mixture, an
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