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  • Title: Stable isotope-enhanced two- and three-dimensional diffusion ordered 13C NMR spectroscopy (SIE-DOSY 13C NMR).
    Author: Vermillion K, Price NP.
    Journal: J Magn Reson; 2009 Jun; 198(2):209-14. PubMed ID: 19303336.
    Abstract:
    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.
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