Combined use of liquid chromatography-nuclear magnetic resonance spectroscopy and liquid chromatography-mass spectrometry for the characterization of an acarbose degradation product

被引：19

作者：

Novak, P ^{[1
]}

Tepes, P ^{[1
]}

Cindric, M ^{[1
]}

Ilijas, M ^{[1
]}

Dragojevic, S ^{[1
]}

Mihaljevic, K ^{[1
]}

机构：

[1] PLIVA Res Inst Ltd, HR-10000 Zagreb, Croatia

来源：

JOURNAL OF CHROMATOGRAPHY A | 2004年 / 1033卷 / 02期

关键词：

nuclear magnetic resonance spectroscopy; acarbose;

D O I：

10.1016/j.chroma.2004.01.055

中图分类号：

Q5 [生物化学];

学科分类号：

071010 [生物化学与分子生物学]; 081704 [应用化学];

摘要：

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 (H-1 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 a-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. (C) 2003 Elsevier B.V. All rights reserved.

引用

页码：299 / 303

页数：5

共 18 条

[1]

ALBERT K, 2002, ONLINE LCNMR RELATED

[2]

CONTROLLED REDUCTION OF ACARBOSE - CONFORMATIONAL-ANALYSIS OF ACARBOSE AND THE RESULTING SATURATED PRODUCTS [J].