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Anal Biochem. 2001 Oct 01;297(1):42-51. doi: 10.1006/abio.2001.5296.

(1)H nuclear magnetic resonance spectroscopic analysis for determination of glucuronic and iduronic acids in dermatan sulfate, heparin, and heparan sulfate.

Analytical biochemistry

M Sudo, K Sato, A Chaidedgumjorn, H Toyoda, T Toida, T Imanari

Affiliations

  1. Graduate School of Pharmaceutical Sciences, Chiba University, Chiba 263-8522, Japan.

PMID: 11567526 DOI: 10.1006/abio.2001.5296

Abstract

(1)H NMR spectroscopy has been established for the determination of uronate residues in glycosaminoglycans (GAGs) such as dermatan sulfate (DS), heparin (HP), and heparan sulfate (HS). Because of variation in the sulfonation positions in DS, HP, or HS, interpretation of spectra is difficult. Solvolysis was applied to remove O-sulfo groups from these GAG chains in dimethyl sulfoxide containing 10% methanol at 80 degrees C for 5 h. In the cases of HP and HS, N-sulfo groups on glucosamine residues were also removed under the same conditions. The resulting unsubstituted amino groups in HP and HS chains were re-N-acetylated using acetic anhydride to obtain homogeneous core structure with the exception of the variation of uronate residues. The contents of glucuronate and iduronate residues in the chemically modified DS, HP, and HS samples were analyzed by 600-MHz (1)H NMR spectroscopy. These methods were applied to compositional analysis of uronate residues in GAGs isolated from various sources.

Copyright 2001 Academic Press.

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