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Chapter 49,969

Practical aspects of ROESY experiments for identification of bound waters in the cyclic tetrasaccharide

Furihata, K.; Fujimoto, T.; Tsutsui, A.; Machinami, T.; Tashiro, M.

Magnetic Resonance in Chemistry: Mrc 43(12): 1044-1048

2005


ISSN/ISBN: 0749-1581
PMID: 16142839
DOI: 10.1002/mrc.1702
Accession: 049968955

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}-alpha-D-Glcp-(1-->3)-alpha-D-Glcp-(1-->6)-alpha-D-Glcp-(1-->3)-alpha-D-Glcp-(1-->).

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