Identification, isolation, and structural characterization of novel forced degradation products of apixaban using advanced analytical techniques.
apixaban
forced degradation studies
high-resolution mass spectrometry
mass spectrometry
ultra-high performance liquid chromatography
Journal
Journal of separation science
ISSN: 1615-9314
Titre abrégé: J Sep Sci
Pays: Germany
ID NLM: 101088554
Informations de publication
Date de publication:
Nov 2022
Nov 2022
Historique:
revised:
17
08
2022
received:
13
06
2022
accepted:
26
08
2022
pubmed:
2
9
2022
medline:
9
11
2022
entrez:
1
9
2022
Statut:
ppublish
Résumé
The current research explains the stress degradation behavior of Apixaban, which is an anticoagulant or blood thinner. The degradation was conducted using hydrolytic, oxidative, thermal, and photolytic conditions. Apixaban is relatively stable in oxidative, thermal, and photolytic conditions; however, considerable degradation was observed in acid and base hydrolysis. Degradation products were identified using ultra-high performance liquid chromatography-mass spectrometry, isolated using semi-preparative high-performance liquid chromatography, and structural characterization by high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy. A total of five degradation products were identified and isolated in acid and base degradation. Degradation products 1, 2, and 3 were observed in acid conditions, whereas in base conditions, along with those three, two more degradation products 4 and 5 were identified. The representative thing was that among the five degradation products, two sets of positional isomers 1, 4, and 2, 5 were observed; out of which 2 and 5 are novel. The remaining degradation products 1, 3, and 4 are already reported tentatively using a single analytical technique of mass analysis without any evidence from nuclear magnetic resonance spectroscopy. Hence, the present study focused on using high-resolution mass, and nuclear magnetic resonance spectroscopy data for concrete confirmation of structures for degradation products.
Identifiants
pubmed: 36048725
doi: 10.1002/jssc.202200466
doi:
Substances chimiques
apixaban
3Z9Y7UWC1J
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
3942-3954Informations de copyright
© 2022 Wiley-VCH GmbH.
Références
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