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A toolbox of HSQC experiments for small molecules at high 13 C‐enrichment. Artifact‐free, fully 13 C‐homodecoupled and J CC ‐encoding pulse sequences
Author(s) -
Foroozandeh Mohammadali,
Giraudeau Patrick,
Jeannerat Damien
Publication year - 2013
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.4019
Subject(s) - heteronuclear single quantum coherence spectroscopy , homonuclear molecule , chemistry , pulse sequence , nuclear magnetic resonance , amplitude , signal (programming language) , modulation (music) , analytical chemistry (journal) , two dimensional nuclear magnetic resonance spectroscopy , molecule , molecular physics , biological system , physics , stereochemistry , optics , organic chemistry , chromatography , computer science , programming language , acoustics , biology
A set of modified HSQC experiments designed for the study of 13 C‐enriched small molecules is introduced. It includes an improved sensitivity‐enhanced HSQC experiment eliminating signal artifacts because of high‐order 13 C magnetization terms generated at high 13 C enrichment. A broadband homonuclear 13 C decoupling sequence based on Zangger and Sterk's method simplifies the complex 13 C– 13 C multiplet structure in the F1 dimension of HSQC. When recording spectra at high resolution, the combination with a multiple‐site modulation of the selective pulse outperforms the constant‐time HSQC in terms of sensitivity and reliability. Finally, two pulse sequences reintroducing selected J CC couplings with selective pulses facilitate their assignments and measurements either in the splitting of the resulting doublets or by modulation of the signal amplitude. A sample of uniformly 92% 13 C‐enriched cholesterol is used as an example. Copyright © 2013 John Wiley & Sons, Ltd.