Stable isotope-enhanced two- and three-dimensional diffusion ordered C NMR spectroscopy (SIE-DOSY C NMR) |
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Authors: | Karl Vermillion Neil PJ Price |
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Institution: | aNew Crops and Processing Technology Research Unit, National Center for Agricultural Utilization Research, Agricultural Research Service, United States Department of Agriculture, 1815 North University Street, Peoria, IL 61604, USA;bBioproducts and Biocatalysis Research Unit, National Center for Agricultural Utilization Research, Agricultural Research Service, United States Department of Agriculture, 1815 North University Street, Peoria, IL 61604, USA |
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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. |
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Keywords: | Stable isotope-enhanced diffusion-ordered spectroscopy DOSY Peracetylation Diffusion Carbohydrate |
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