High-resolution four-dimensional carbon-correlated 1H-1H ROESY experiments employing isotags and the filter diagonalization method for effective assignment of glycosidic linkages in oligosaccharides

Journal of Magnetic Resonance
Geoffrey S Armstrong, Brad Bendiak

Abstract

Four-dimensional nuclear magnetic resonance spectroscopy of oligosaccharides that correlates 1H-1H ROESY cross peaks to two additional 13C frequency dimensions is reported. The 13C frequencies were introduced by derivatization of all free hydroxyl groups with doubly 13C-labeled acetyl isotags. Pulse sequences were optimized for processing with the filter diagonalization method. The extensive overlap typically observed in 2D ROESY 1H-1H planes was alleviated by resolution of ROESY cross peaks in the two added dimensions associated with the carbon frequencies of the isotags. This enabled the interresidue 1H-1H ROESY cross peaks to be unambiguously assigned hence spatially proximate sugar spin systems across glycosidic bonds could be effectively ascertained. An experiment that selectively amplifies interresidue ROESY 1H-1H cross peaks is also reported. It moves the magnetization of an intraresidue proton normally correlated to a sugar H-1 signal orthogonally along the z axis prior to a Tr-ROESY mixing sequence. This virtually eliminates the incoherent intraresidue ROESY transfer, suppresses coherent TOCSY transfer, and markedly enhances the intensity of interresidue ROESY cross peaks.

References

Mar 1, 1995·Journal of Magnetic Resonance. Series B·E KupceI D Campbell
Nov 1, 1995·Journal of Biomolecular NMR·F DelaglioA Bax
Dec 24, 1997·Clinical Science·E F HounsellM J Davies
Aug 26, 1998·Journal of Magnetic Resonance·V A MandelshtamA J Shaka
Jul 20, 1999·Annual Review of Biophysics and Biomolecular Structure·C A BushA Imberty
Dec 2, 1999·Biochimica Et Biophysica Acta·T Hennet, L G Ellies
Apr 12, 2002·Journal of Magnetic Resonance·Kristin E CanoA J Shaka
Sep 12, 2002·Biochimica Et Biophysica Acta·Hans-Joachim GabiusHans-Christian Siebert
Sep 2, 2003·Angewandte Chemie·Michael J Thrippleton, James Keeler
Apr 6, 2005·Journal of Magnetic Resonance·Geoffrey S Armstrong, Brad Bendiak

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Citations

Dec 26, 2007·Biochimica Et Biophysica Acta·Koichi KatoYoshiki Yamaguchi
Apr 11, 2015·Evidence-based Complementary and Alternative Medicine : ECAM·Xiang-Yang ChenBin Liu
Dec 11, 2014·Journal of the American Society for Mass Spectrometry·Yanglan Tan, Nicolas C Polfer
Jan 5, 2017·Journal of the American Society for Mass Spectrometry·Yanglan TanNicolas C Polfer

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