Stable isotope-enhanced two- and three-dimensional diffusion ordered 13C NMR spectroscopy (SIE-DOSY 13C NMR).
The feasibility of obtaining high quality homonuclear or heteronuclear diffusion-ordered (13)C NMR data is shown to be greatly improved by using (13)C isotopically-enriched samples. Stable isotope-enhanced diffusion ordered (SIE-DOSY) (13)C NMR has been applied to (13)C-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-(13)C]xylose, [U-(13)C]glucose, and [1-(13)C(gal)]lactose were obtained in 5h. Sample derivatization with [carbonyl-(13)C]acetate (peracetylation) extends the usefulness of the technique to included non-labeled sugars; the (13)C-carbonyl - carbohydrate ring proton (1)H-(13)C correlations also provide additional structural information, as shown for the 3-D DOSY-HMQC analysis of a mixture of maltotriose and lactose per-[carbonyl-(13)C]acetates.
Vermillion
Karl
K
New Crops and Processing Technology Research Unit, National Center for Agricultural Utilization Research, Agricultural Research Service, United States Department of Agriculture, Peoria, IL 61604, USA. karl.vermillion@ars.usda.gov
Price
Neil P J
NP
D000085:Acetates / Q000737:chemistry; D000107:Acetylation; D002241:Carbohydrates / Q000737:chemistry*; D004058:Diffusion; D004187:Disaccharides / Q000737:chemistry; D005947:Glucose / Q000737:chemistry; D006601:Hexoses / Q000737:chemistry; D007553:Isotope Labeling; D007785:Lactose / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D010429:Pentoses / Q000737:chemistry; D014994:Xylose / Q000737:chemistry
D000085:Acetates; D002241:Carbohydrates; D004187:Disaccharides; D006601:Hexoses; D010429:Pentoses; D014994:Xylose; D005947:Glucose; D007785:Lactose