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3D Heteronuclear long-range 1H–13C scalar correlation at natural abundance: application to oligosaccharide analysis

✍ Scribed by Griselda Hernández; David M. LeMaster

Publisher
John Wiley and Sons
Year
2002
Tongue
English
Weight
246 KB
Volume
40
Category
Article
ISSN
0749-1581

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✦ Synopsis

Abstract

A 3D ^1^H–^13^C–^1^H refocused INEPT transfer experiment is proposed in which the initial coherence transfer of ^1^H longitudinal to ^13^C transverse magnetization is tuned to the long‐range ^1^H, ^13^C couplings while the reverse INEPT component transfers the magnetization to the directly bonded ^1^H. Integration of a constant time ^1^H evolution period into the long‐range coherence transfer interval provides absorption mode signals for each dimension. A ^13^C purge component at the beginning of the sequence selects for ^12^C‐bound ^1^H magnetization that is then transferred to a ^13^C‐bound hydrogen, thus strongly suppressing the diagonal signals. This experiment is expected to be of particular value for situations in which resonance overlap in the ^13^C dimension renders 2D long‐range heteronuclear correlation data ambiguous. In combination with a diagonal‐suppressed 3D ^1^H–^13^C–^1^H TOCSY‐HSQC experiment, complete assignment of the ring resonances of the Lewis‐b hexasaccharide was obtained on a 4.2 mM sample using a conventional 500 MHz probe (0.1% ethylbenzene signal‐to‐noise ratio of 600), suggesting its applicability to sub‐millimolar samples using cryoprobe technology. Copyright © 2002 John Wiley & Sons, Ltd.

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