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Identification of impurities in acarbose by using an integrated liquid chromatography‐nuclear magnetic resonance and liquid chromatography‐mass spectrometry approach

2005; Wiley; Volume: 28; Issue: 13 Linguagem: Inglês

10.1002/jssc.200400057

1615-9314

Predrag Novak, Mario Cindrić, Predrag Tepeš, Snježana Dragojević, Marina Ilijaš, Krešo Mihaljević,

Metabolomics and Mass Spectrometry Studies

Abstract 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.