A detailed structural analysis of the copolyesterification in bulk without any external catalyst at 160ЊC between o-phthalic anhydride (P), oleic acid (O), and trimethylolpropane (T) with a mol ratio ([{COOH]/[{OH]) Å 0.70 has been carried out by high resolution 13 C nuclear magnetic resonance ( 13
1H Nuclear Magnetic Resonance Spectroscopic Analysis for Determination of Glucuronic and Iduronic Acids in Dermatan Sulfate, Heparin, and Heparan Sulfate
✍ Scribed by Masahiro Sudo; Kenji Sato; Amornrut Chaidedgumjorn; Hidenao Toyoda; Toshihiko Toida; Toshio Imanari
- Publisher
- Elsevier Science
- Year
- 2001
- Tongue
- English
- Weight
- 114 KB
- Volume
- 297
- Category
- Article
- ISSN
- 0003-2697
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✦ Synopsis
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°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.
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