NMR Experiments for the Measurement of Proton-proton and Carbon-carbon Residual Dipolar Couplings in Uniformly Labelled Oligosaccharides

Overview

Journal J Biomol NMR

Publisher Springer

Specialties Molecular Biology
Nuclear Medicine

Date 2003 Jun 20

PMID 12815261

Citations 3

Authors

Manuel Martin-Pastor

Angeles Canales-Mayordomo

Jesus Jimenez-Barbero

Affiliations

Soon will be listed here.

Abstract

A 2D-HSQC-carbon selective/proton selective-constant time COSY, 2D-HSQC-(sel C, sel H)-CT COSY experiment, which is applicable to uniformly (13)C isotopically enriched samples (U-(13)C) of oligosaccharides or oligonucleotides is proposed for the measurement of proton-proton RDC in crowded regions of 2D-spectra. In addition, a heteronuclear constant time-COSY experiment, (13)C-(13)C CT-COSY, is proposed for the measurement of one bond carbon-carbon RDC in these molecules. These two methods provide an extension, to U-(13)C molecules, of the original homonuclear constant time-COSY experiment proposed by Tian et al. (1999) for saccharides. The combination of a number of these RDC with NOE data may provide the method of choice to study oligosaccharide conformation in the free and receptor-bound state.

Citing Articles

NMR structure analysis of uniformly 13C-labeled carbohydrates.

Fontana C, Kovacs H, Widmalm G J Biomol NMR. 2014; 59(2):95-110.

PMID: 24771296 DOI: 10.1007/s10858-014-9830-6.

Realizing the Promise of Chemical Glycobiology.

Wang L, Davis B Chem Sci. 2013; 4(9):3381-3394.

PMID: 23914294 PMC: 3731165. DOI: 10.1039/C3SC50877C.

Structural monitoring of oligosaccharides through 13C enrichment and NMR observation of acetyl groups.

Yu F, Prestegard J Biophys J. 2006; 91(5):1952-9.

PMID: 16782783 PMC: 1544292. DOI: 10.1529/biophysj.105.079913.

References

Kupce E, Boyd J, Campbell I . Short selective pulses for biochemical applications. J Magn Reson B. 1995; 106(3):300-3. DOI: 10.1006/jmrb.1995.1049. View

Fischer M, Losonczi J, Weaver J, Prestegard J . Domain orientation and dynamics in multidomain proteins from residual dipolar couplings. Biochemistry. 1999; 38(28):9013-22. DOI: 10.1021/bi9905213. View

Garcia-Herrero A, Montero E, Munoz J, Espinosa J, Vian A, Garcia J . Conformational selection of glycomimetics at enzyme catalytic sites: experimental demonstration of the binding of distinct high-energy distorted conformations of C-, S-, and O-glycosides by E. Coli beta-galactosidases. J Am Chem Soc. 2002; 124(17):4804-10. DOI: 10.1021/ja0122445. View

Prestegard J . New techniques in structural NMR--anisotropic interactions. Nat Struct Biol. 1998; 5 Suppl:517-22. DOI: 10.1038/756. View

Freedberg D . An alternative method for pucker determination in carbohydrates from residual dipolar couplings: a solution NMR study of the fructofuranosyl ring of sucrose. J Am Chem Soc. 2002; 124(10):2358-62. DOI: 10.1021/ja010981v. View

Dwek R . Glycobiology: Toward Understanding the Function of Sugars. Chem Rev. 1996; 96(2):683-720. DOI: 10.1021/cr940283b. View

Tian F, Craighead J, Prestegard J . Conformational analysis of a flexible oligosaccharide using residual dipolar couplings. J Am Chem Soc. 2001; 123(3):485-92. DOI: 10.1021/ja002900l. View

Martin-Pastor M, Bush C . Refined structure of a flexible heptasaccharide using 1H-13C and 1H-1H NMR residual dipolar couplings in concert with NOE and long range scalar coupling constants. J Biomol NMR. 2001; 19(2):125-39. DOI: 10.1023/a:1008327926009. View

Asensio J, Canada F, Jimenez-Barbero J . Studies of the bound conformations of methyl alpha-lactoside and methyl beta-allolactoside to ricin B chain using transferred NOE experiments in the laboratory and rotating frames, assisted by molecular mechanics and dynamics calculations. Eur J Biochem. 1995; 233(2):618-30. DOI: 10.1111/j.1432-1033.1995.618_2.x. View

10.

Wu Z, Bax A . Measurement of homonuclear proton couplings based on cross-peak nulling in CT-COSY. J Magn Reson. 2001; 151(2):242-52. DOI: 10.1006/jmre.2001.2358. View

11.

Tian F, Fowler C, Zartler E, Jenney Jr F, Adams M, Prestegard J . Direct measurement of 1H-1H dipolar couplings in proteins: a complement to traditional NOE measurements. J Biomol NMR. 2000; 18(1):23-31. DOI: 10.1023/a:1008384904380. View

12.

Azurmendi H, Bush C . Tracking alignment from the moment of inertia tensor (TRAMITE) of biomolecules in neutral dilute liquid crystal solutions. J Am Chem Soc. 2002; 124(11):2426-7. DOI: 10.1021/ja017524z. View

13.

Tjandra N, Bax A . Direct measurement of distances and angles in biomolecules by NMR in a dilute liquid crystalline medium. Science. 1997; 278(5340):1111-4. DOI: 10.1126/science.278.5340.1111. View