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Applications of cryogenic NMR probe technology to long‐range 1 H‐ 15 N 2D NMR studies at natural abundance
Author(s) -
Crouch Ronald C.,
Llanos William,
Mehr Knut G.,
Hadden Chad E.,
Russell David J.,
Martin Gary E.
Publication year - 2001
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.886
Subject(s) - chemistry , analytical chemistry (journal) , spectrometer , nuclear magnetic resonance spectroscopy , natural abundance , resonance (particle physics) , proton nmr , nuclear magnetic resonance , range (aeronautics) , mass spectrometry , atomic physics , chromatography , physics , stereochemistry , optics , materials science , composite material
Abstract The development of new NMR probe technologies has been an active area of research effort for the past decade. Recently, cryogenically cooled NMR probes have been the subject of considerable interest in the light of the large gains in sensitivity and hence savings in spectrometer time that can be realized by utilizing this technology. With low gamma nuclides, such as 15 N, time savings may be less of an issue than the ability to work with available samples rather than having to isolate additional material for analysis. Results of 5–10 Hz optimized CIGAR‐HMBC 1 H– 15 N experiments at natural abundance obtained using a 5 mm Varian 1 H– 15 N Cryo‐Q NMR probe are compared with those from a 3 mm gradient inverse triple resonance probe using a 2 mg sample of the oxazolidinone antibiotic eperezolid in a 3 mm NMR tube. Using the cryogenic NMR probe, a 1 H– 15 N CIGAR‐HMBC spectrum in which most previously reported long‐range couplings are observed was recorded in ∼10 min; almost all of the expected long‐range responses were observed within 26 min. Acquiring the same data set with identical parameters using a conventional 3 mm gradient inverse triple resonance probe gave data that were of substantially lower quality. Acquiring data comparable to the 26 min cryogenic probe data with the conventional 3 mm probe required ∼4 h to observe all of the responses and ∼18 h to obtain a spectrum with a signal‐to‐noise ratio comparable to the data set acquired with the cryogenic NMR probe. Copyright © 2001 John Wiley & Sons, Ltd.