Stable isotope-enhanced two- and three-dimensional diffusion ordered 13C NMR spectroscopy (SIE-DOSY 13C NMR)

Abstract

The feasibility of obtaining high quality homonuclear or heteronuclear diffusion-ordered 13C NMR data is shown to be greatly improved by using 13C isotopically-enriched samples. Stable isotope-enhanced diffusion ordered (SIE-DOSY) 13C NMR has been applied to 13C-enriched carbohydrates, and has been used to determine diffusion coefficients for pentose and hexose monosaccharides, and a disaccharide and trisaccharide. These 2D spectra were obtained with as little as 8 min of acquisition time. Fully resolved 3D DOSY-HMQC NMR spectra of [U-13C]xylose, [U-13C]glucose, and [1-13Cgal]lactose were obtained in 5 h. Sample derivatization with [carbonyl-13C]acetate (peracetylation) extends the usefulness of the technique to included non-labeled sugars; the 13C-carbonyl - carbohydrate ring proton 1H-13C correlations also provide additional structural information, as shown for the 3-D DOSY-HMQC analysis of a mixture of maltotriose and lactose per-[carbonyl-13C]acetates. © 2009 Elsevier Inc. All rights reserved.