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Identification of impurities in acarbose by using an integrated liquid chromatography‐nuclear magnetic resonance and liquid chromatography‐mass spectrometry approach
Author(s) -
Novak Predrag,
Cindrić Mario,
Tepeš Predrag,
Dragojević Snježana,
Ilijaš Marina,
Mihaljević Krešo
Publication year - 2005
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200400057
Subject(s) - acarbose , chemistry , chromatography , mass spectrometry , liquid chromatography–mass spectrometry , impurity , nuclear magnetic resonance spectroscopy , analytical chemistry (journal) , stereochemistry , organic chemistry , enzyme
The usefulness of applying an integrated LC‐NMR and LC‐MS approach to acarbose bulk drug impurity profiling is demonstrated. LC‐MS and LC‐NMR methodologies were employed for the online separation and structural elucidation of a final drug product. Combining data provided by the stop‐flow LC‐NMR and LC‐MS experiments made it possible to identify the main components present in the acarbose sample. Spectral analysis revealed that A and B were known impurities while C was an unknown compound. LC‐MS and LC‐NMR analyses revealed that C was a pentasaccharide differing from the acarbose in number and nature of sugar subunits in the molecule. It was subsequently isolated and its structure was confirmed by the offline 1‐ and 2‐D NMR experiments, and atom assignment was made.