Limtiaco, J. F. K. and Béni, Szabolcs and Jones, C. J. and Langeslay, D. J. and Larive, Cynthia K. (2011) The efficient structure elucidation of minor components in heparin digests using microcoil NMR. Carbohydrate Research, 346 (14). pp. 2244-2254. ISSN 0008-6215
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Abstract
The structural complexity and microheterogeneity of the glycosaminoglycans heparin and heparan sulfate make their characterization a daunting task. The methodology described herein utilizes a combination of enzymatic digestion, size-exclusion chromatography, strong anion-exchange HPLC, reverse-phase ion-pair ultrahigh performance liquid chromatography-mass spectrometry, and microcoil NMR for the efficient sequencing of heparin-derived tetrasaccharides. The high mass sensitivity of microcoil NMR makes this technique well suited for the characterization of mass-limited samples removing a bottleneck in the analysis workflow and permitting structural characterization of minor components isolated from a heparin enzymatic digestion. Complete characterization of one tetrasulfonated, five pentasulfonated isomers and two hexasulfonated tetrasaccharide sequences is described. To our knowledge, two of the identified minor tetrasaccharides are unique, and have not been previously reported: IdoA(2S)-GlcNS(6S)-IdoA(2S)-GlcNS(6S) and ΔUA(2S)-GlcNS(6S)-IdoA-GlcNS(6S) . © 2011 Elsevier Ltd. All rights reserved.
Item Type: | Article |
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Uncontrolled Keywords: | ultra performance liquid chromatography; reversed phase high performance liquid chromatography; priority journal; Nuclear magnetic resonance spectroscopy; nonhuman; gel permeation chromatography; enzyme metabolism; DEPOLYMERIZATION; carbohydrate analysis; ARTICLE; aqueous solution; anion exchange; animal experiment; tetrasaccharide; HEPARIN; heparan sulfate; Size exclusion chromatography; RESONANCE; Polysaccharides; Mass Spectrometry; ISOMERS; Ion exchange; high performance liquid chromatography; Data communication equipment; characterization; Tetrasaccharides; DIASTEREOMERS; UPLC-MS; Unsaturated tetrasaccharide; nuclear magnetic resonance; Microcoil NMR; Hexuronic acid epimers; Heparin diastereomers |
Subjects: | R Medicine / orvostudomány > RM Therapeutics. Pharmacology / terápia, gyógyszertan |
SWORD Depositor: | MTMT SWORD |
Depositing User: | MTMT SWORD |
Date Deposited: | 16 Feb 2016 10:27 |
Last Modified: | 16 Feb 2016 10:27 |
URI: | http://real.mtak.hu/id/eprint/33470 |
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