High-resolution H-NMR Spectroscopy

The recent development of high-field NMR spectrometers with increased resolution, dynamic range and 

Grootveld et al. (1994) employed this technique to investigate radiolytic, damage to biomolecules present in human body fluids. 7-Radiolysis of healthy or rheumatoid human serum (5.00 kGy) in the presence of atmospheric O2 gave rise to reproducible elevations in the concentration of NMR-detectable acetate, which are predominantly ascribable to the prior oxidation of lactate to pyruvate by OH radical followed by oxidative decarboxylation of pyruvate by radiolytically generated H2O2 and/or further OH radicals (Equations 1.7 and 1.8). 

Typical spectra obtained are shown in Fig. 1.2. Moreover, substantial radiolytically-mediated elevations in the concentration of serum formate, arising from the oxidation of carbohydrates present by OH radical, were also detectable. In addition to the above modifications, 7-radiolysis of inflammatory knee-joint synovial fluid generated an oligosaccharide species of low molecular mass derived from the radiolytic fragmentation of hyaluronate as outlined in the previous section dealing with oxidative damage to carbohydrates. The 

Exposure of the amino acid methionine to H2O2 or an OH radical flux generates methionine sulphoxide as a 

We have recently applied high-resolution H-NMR spectroscopy to demonstrate the oxidative consumption of salivary pyruvate by this product (Fig. 1.6), a reaction consistent with Equation 1.11 (Lynch et al., unpublished data). 

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The applications of high-resolution H-NMR spectroscopy to the analysis of products arising from the lipid peroxidation process are described in Section 7. 

The macrocycle l,4,7,10-tetraazacyclododecane-N,N, N",N" -tetraacetic acid (DOTA) is known to form stable complexes with lanthanides. A steroid conjugate (Fig. 8.16) was prepared via coupling of 6a-amino-17p-estradiol with a C functionalized DOTA derivative, namely, p-thiocyanatobenzyl DOTA, as a BFCA. The synthesis of 6a-amino-17p-estradiol was carried out by a four step reaction sequence. The intermediate and target compounds were characterized using high resolution H-NMR spectroscopy. 

Bollard, M.E, Holmes, E. Lindon, J.C. Mitchell, S.C. Branstetter, D. Zhang, W. Nicholson, J.K. Investigations into Biochemical Changes Due to Diurnal Variation and Estrus Cycle in Female Rats Using High Resolution H NMR Spectroscopy of Urine and Pattern Recognition, Anal. Biochem. 295, 194-202 (2001). 

The ee of the alcohol was determined by analysis of the corresponding Mosher ester derivative by high resolution h NMR spectroscopy (400 MHz. CeDs). The preparation of the Mosher ester is described below. 

Caligiani, A., Acquotti, D., PaUa, G., and Bocchi, V, Identification and quantification of the main organic components of vinegars by high resolution H NMR spectroscopy. Anal. Chim. Acta, 585,110-119, 2007. 

C. Coelho, J. Rocha, P.K. Madhu, L. Mafia, Practical aspects of Lee—Goldburg based CRAMPS techniques for high-resolution H NMR spectroscopy in solids implementation and apphcations, J. Magn. Reson. 194 (2) (2008) 264—282. 

Riemer, T., Nimptsch, A., Nimptsch, K., and Schiller, J. 2012. Determination of the glycosaminoglycan and collagen contents in tissue samples by high-resolution H NMR spectroscopy after DCl-induced hydrolysis. Biomacromolecules, 13 2110-2117. 

I. SchneU, H.W. Spiess, High-resolution H NMR spectroscopy in the solid state very st sample rotation and multiple-quantum coherences, J. Magn. Reson. 151 (2001) 153-227. 

Wevers RA, Engelke U, Heerschap A. High-resolution H-NMR spectroscopy of blood plasma for metabolic studies. Clin Chem 1994 40 1245-1250. 

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