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Practical aspects of ROESY experiments for identification of bound waters in the cyclic tetrasaccharide
Author(s) -
Furihata Kazuo,
Fujimoto Takashi,
Tsutsui Ayumi,
Machinami Tomoya,
Tashiro Mitsuru
Publication year - 2005
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1702
Subject(s) - tetrasaccharide , chemistry , pulse sequence , pulse (music) , stereochemistry , excitation , nuclear magnetic resonance , organic chemistry , optics , physics , polysaccharide , quantum mechanics , detector
ROESY pulse sequences are presented and evaluated to identify bound waters in the cyclic tetrasaccharide. The first experiment incorporated the double‐pulsed field gradient spin‐echo (DPFGSE) for selective water excitation at the initial portion of the pulse sequence. Although long, shaped pulses were used in DPFGSE to achieve the highly selective excitation of water resonance that is very close to resonances of the cyclic tetrasaccharide, the approach was not effective because of the loss of sensitivity. Concomitant use of long delays and moderate length of shaped pulses in the portion of DPFGSE gained more sensitivity. A simple approach incorporating spin‐echo with long delays instead of DPFGSE also afforded a sensitive spectrum. Practical aspects of these ROESY experiments are illustrated using the cyclic tetrasaccharide cyclo ‐{→6}‐α‐ D ‐Glc p ‐(1→3)‐α‐ D ‐Glc p ‐(1→6)‐α‐ D ‐Glc p ‐(1→3)‐α‐ D ‐Glc p ‐(1→). Copyright © 2005 John Wiley & Sons, Ltd.