(3, 2)D 1H, 13C BIRDr,X-HSQC-TOCSY for NMR Structure Elucidation of Mixtures. Application to Complex Carbohydrates

Dusan Uhrin, Natalia Brodaczewska, Zuzana Košťálová

Research output: Contribution to journalArticlepeer-review

Abstract

Overlap of NMR signals is the major cause of difficulties associated with NMR structure elucidation of molecules contained in complex mixtures. A 2D homonuclear correlation spectroscopy in particular suffers from low dispersion of 1H chemical shifts; larger dispersion of 13C chemical shifts is often used to reduce this overlap, while still providing the proton–proton correlation information e.g. in the form of a 2D 1H, 13C HSQC-TOCSY experiment. For this methodology to work, 13C chemical shift must be resolved. In case of 13C chemical shifts overlap, 1H chemical shifts can be used to achieve the desired resolution. The proposed (3, 2)D 1H, 13C BIRDr,X-HSQC-TOCSY experiment achieves this while preserving singlet character of cross peaks in the F1 dimension. The required high-resolution in the 13C dimension is thus retained, while the cross peak overlap occurring in a regular HSQC-TOCSY experiment is eliminated. The method is illustrated on the analysis of a complex carbohydrate mixture obtained by depolymerisation of a fucosylated chondroitin sulfate isolated from the body wall of the sea cucumber Holothuria forskali.
Original languageEnglish
JournalJournal of Biomolecular Nmr
Early online date11 Jan 2018
DOIs
Publication statusE-pub ahead of print - 11 Jan 2018

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