Naslov
Identification of impurities in acarbose by using an integrated liquid chromatography-nuclear magnetic resonace and liquid chromatography-mass spectrometry approach

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

Izvornik
Journal of separation science (1615-9306) 28 (2005), 13; 1442-1447

Vrsta, podvrsta i kategorija rada
Radovi u časopisima, članak, znanstveni

Ključne riječi
acarbose; impurities; liquid chromatography-nuclear magnetic resonance spectroscopy; liquid chromatography-mass spectrometry

Sažetak
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 on-line 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 pentasacharide differing from the acarbose in a number and nature of sugar subunits in the molecule. It was subsequently isolated and its structure was confirmed by the off-line one- and two-dimensional NMR experiments and atom assignment was made.

Izvorni jezik
Engleski

Znanstvena područja
Kemija

POVEZANOST RADA