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

被引:0
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作者
Ishii-Karakasa, I [1 ]
机构
[1] Kitasato Univ, Dept Biochem, Sch Med, Kanagawa 2288555, Japan
关键词
oligosaccharide; nanomole order analysis; 1D H-1-NMR; H-HCOSY; full-assignment;
D O I
暂无
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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 oligosaccharide 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 oligosaccharide 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 protons included in overlapped peaks is from the tripler to the octet (dd-ddd). 3. In the oligosaccharide, the conformations of composite monosaccharides are similar to those of the corresponding monosaccharide derivatives. The program (FORTRAN 77) for an analysis under this condition was developed, and was applied to analyses of pyridylaminated-disaccharide (Gal beta1-3GalNAc-PA) and disaccharide-alditol (Gal beta1-3GalNAc-ol).
引用
收藏
页码:319 / 327
页数:9
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