Enantioseparation of 2-(4-chlorophenyl)succinic acid by countercurrent chromatography and investigation of injection volume on resolution.
countercurrent chromatography
enantioseparation
injection volume
resolution
Journal
Journal of separation science
ISSN: 1615-9314
Titre abrégé: J Sep Sci
Pays: Germany
ID NLM: 101088554
Informations de publication
Date de publication:
Feb 2021
Feb 2021
Historique:
received:
08
08
2020
revised:
01
11
2020
accepted:
24
11
2020
pubmed:
29
11
2020
medline:
29
11
2020
entrez:
28
11
2020
Statut:
ppublish
Résumé
2-(4-Chlorophenyl)succinic acid was successfully enantioseparated by countercurrent chromatography using hydroxypropyl-β-cyclodextrin as chiral selector. A two-phase solvent system composed of n-hexane-ethyl acetate-0.1 mol/L phosphate buffer with pH 2.65 (5:5:10, v/v) was selected. Enantioselective liquid-liquid extraction was used to optimize the enantioseparation conditions. Meanwhile, the influence of injection volume on resolution in countercurrent chromatography was investigated and a linear relationship between the inflection point of injection volume and sample loading was tentatively obtained. The peak resolution will decrease significantly when the injection volume over the inflection point was used. In addition, it could be found that the smaller amount of sample loading, the larger impact of injection volume on resolution could be observed, which might serve as a good reference for the selection of sample volume in enantioseparations by countercurrent chromatography. Under optimized conditions, 20 mg of 2-(4-chlorophenyl)succinic acid racemate dissolved in 10 mL of aqueous phase was successfully enantioseparated by countercurrent chromatography. The recovery for both of the enantiomer of (±)-2-(4-chlorophenyl)succinic acid reached within 70-75% with a purity of 99.0%.
Identifiants
pubmed: 33247875
doi: 10.1002/jssc.202000860
doi:
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
752-758Informations de copyright
© 2020 Wiley-VCH GmbH.
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