Convenient method for a full-assignment of the H-1-NMR spectrum of oligosaccharide

Citation
I. Ishii-karakasa, Convenient method for a full-assignment of the H-1-NMR spectrum of oligosaccharide, BUNSEKI KAG, 50(5), 2001, pp. 319-327
Citations number
7
Categorie Soggetti
Spectroscopy /Instrumentation/Analytical Sciences
Journal title
BUNSEKI KAGAKU
ISSN journal
05251931 → ACNP
Volume
50
Issue
5
Year of publication
2001
Pages
319 - 327
Database
ISI
SICI code
0525-1931(200105)50:5<319:CMFAFO>2.0.ZU;2-5
Abstract
Measurements of the 600 MHz 1D H-1-NMR and H-H COSY spectra are possible at the nanomole order of oligosaccharide. However, many proton peaks of oligo saccharide are observed to overlap at near delta 2 similar to 4 ppm in the H-1-NMR spectrum. Therefore, full assignments of the H-1-NMR spectrum of ol igosaccharide are difficult from only the ID H-1-NMR and H-H COSY spectral data. However an analysis of the H-1-NMR spectrum of the oligosaccharide is possible using the following three conditions: I. The splitting pattern of the AMX type is symmetric at the chemical shift. 2. The multiplicity of pr otons included in overlapped peaks is from the tripler to the octet (dd-ddd ). 3. In the oligosaccharide, the conformations of composite monosaccharide s are similar to those of the corresponding monosaccharide derivatives. The program (FORTRAN 77) for an analysis under this condition was developed, a nd was applied to analyses of pyridylaminated-disaccharide (Gal beta1-3GalN Ac-PA) and disaccharide-alditol (Gal beta1-3GalNAc-ol).