Increasing sensitivity and versatility in NMR supersequences with new HSQC-based modules

Jonathan R J Yong; Alexandar L Hansen; Ēriks Kupče; Tim D W Claridge

doi:10.1016/j.jmr.2021.107027

Increasing sensitivity and versatility in NMR supersequences with new HSQC-based modules

J Magn Reson. 2021 Aug:329:107027. doi: 10.1016/j.jmr.2021.107027. Epub 2021 Jun 19.

Authors

Jonathan R J Yong¹, Alexandar L Hansen², Ēriks Kupče³, Tim D W Claridge⁴

Affiliations

¹ Chemistry Research Laboratory, Department of Chemistry, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK.
² Campus Chemical Instrument Center, The Ohio State University, 460 W. 12th Avenue, Columbus, OH 43210, USA.
³ Bruker UK Ltd., Banner Lane, Coventry CV4 9GH, UK.
⁴ Chemistry Research Laboratory, Department of Chemistry, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. Electronic address: tim.claridge@chem.ox.ac.uk.

PMID: 34246882
DOI: 10.1016/j.jmr.2021.107027

Abstract

The sensitivity-enhanced HSQC, as well as HSQC-TOCSY, experiments have been modified for incorporation into NOAH (NMR by Ordered Acquisition using ¹H detection) supersequences, adding diversity for ¹³C and ¹⁵N modules. Importantly, these heteronuclear modules have been specifically tailored to preserve the magnetisation required for subsequent acquisition of other heteronuclear or homonuclear modules in a supersequence. In addition, we present protocols for optimally combining HSQC and HSQC-TOCSY elements within the same supersequences, yielding high-quality 2D spectra suitable for structure characterisation but with greatly reduced experiment durations. We further demonstrate that these time savings can translate to increased detection sensitivity per unit time.

Keywords: Analytical methods; HSQC-TOCSY; NMR spectroscopy; NOAH supersequences; Sensitivity-enhanced HSQC.

Publication types

Research Support, Non-U.S. Gov't