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Low‐level long‐range 1 H– 15 N heteronuclear shift correlation at natural abundance using a combination of 2D and selective 1D NMR methods with submicro NMR probe technology
Author(s) -
Hadden Chad E.,
Martin Gary E.
Publication year - 1999
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/(sici)1097-458x(199905)37:5<385::aid-mrc480>3.0.co;2-a
Subject(s) - heteronuclear molecule , chemistry , heteronuclear single quantum coherence spectroscopy , abundance (ecology) , analytical chemistry (journal) , carbon 13 nmr , fluorine 19 nmr , proton nmr , two dimensional nuclear magnetic resonance spectroscopy , nuclear magnetic resonance , nuclear magnetic resonance spectroscopy , chromatography , stereochemistry , physics , fishery , biology
Abstract There has been burgeoning interest in the utilization of 15 N as a structural probe. A growing body of reports have appeared using gradient long‐range 1 H– 15 N heteronuclear shift correlation experiments at natural abundance. The majority of studies have reported data acquired using conventional 5 mm NMR probe technology, which has mandated the use of sizable samples to maintain appropriate working concentrations to keep data acquisition times manageable. This paper reports the combined utilization of gradient 2D and selective 1D 1 H– 15 N GHMBC NMR methods in conjunction with SMIDG (submicro inverse‐detection gradient) NMR probe technology at 600 MHz which allows the acquisition of high quality, long‐range natural abundance 1 H– 15 N heteronuclear shift correlation data on samples as small as 1 µmol in 22 h and 0.5 µmol over a long weekend (84 h). In contrast, using 2D NMR methods alone, data on a 1 µmol sample of strychnine acquired over a weekend (65 h) are still of marginal quality. Copyright © 1999 John Wiley & Sons, Ltd.