Combined use of liquid chromatography-nuclear magnetic resonance spectroscopy and liquid chromatography-mass spectrometry for the characterization of an acarbose degradation product |
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Authors: | Novak Predrag Tepes Predrag Cindrić Mario Ilijas Marina Dragojević Snjezana Mihaljević Kreso |
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Affiliation: | Department of Chemistry, University of North Carolina, Greensboro, Greensboro, NC 27403, USA. |
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Abstract: | Directly coupled LC-MS and LC-NMR were applied to identify and structurally characterize an acarbose degradation product A in acidic media. A comparative analysis of the stop-flow LC-NMR (1H and TOCSY) and LC-MS data provided evidence that A is structurally related to acarbose, differing from the parent compound in a number of subunits present in the molecule. Spectral analysis revealed that A was the alpha-glucosidase inhibitor amylostatin XG. Complementary information obtained from the two methods led to the structural elucidation of A which was later corroborated by high-resolution NMR spectroscopy of the isolated molecule. |
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Keywords: | Nuclear magnetic resonance spectroscopy Acarbose |
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