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New N.M.R.-spectroscopic approaches for structural studies of polysaccharides: Application to the Haemophilus influenzae type a capsular polysaccharide

✍ Scribed by R.Andrew Byrd; William Egan; Michael F. Summers; Ad Bax


Publisher
Elsevier Science
Year
1987
Tongue
English
Weight
800 KB
Volume
166
Category
Article
ISSN
0008-6215

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✦ Synopsis


The extension of several modern nuclear magnetic resonance (n.m.r.) spectroscopic techniques to polysaccharides is discussed and illustrated, using the native Haemophilus influenzue type a capsular polysaccharide. These techniques provide for the unambiguous assignment of all n.m.r. resonances ('H, 13C, and 31P) via high-sensitivity homonuclear and 'H-detected heteronuclear correlations, and they are capable of locating the intersaccharide linkages (both O-linked and phosphoric diester-linked) and appended groups (e.g. 0-acetyl groups). To illustrate the power and sensitivity of these methods, a lo-mg sample of the H. Influenzae type a polysaccharide (repeat unit mol. wt. = 376) was studied. The combined acquisition time for the two-dimensional lHJ3C correlation data (one-bond and multiple-bond), the lHJIP correlation data, and the 'H-'H (homonuclear Hartmann-Hahn) data was -18 h.