NMR Research Today is a free monthly online journal that collates and summarizes the latest research about NMR, including details on nuclear magnetic resonance, structural determination, techniques. | ||||||
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PASADENA hyperpolarization of succinic acid for MRI and NMR spectroscopy.Chekmenev EY, Hövener J, Norton VA, Harris K, Batchelder LS, Bhattacharya P, Ross BD, Weitekamp DP A. A. Noyes Laboratory of Chemical Physics, California Institute of Technology, Pasadena, California 91125, USA. We use the PASADENA (parahydrogen and synthesis allow dramatically enhanced nuclear alignment) method to achieve 13C polarization of approximately 20% in seconds in 1-13C-succinic-d2 acid. The high-field 13C multiplets are observed as a function of pH, and the line broadening of C1 is pronounced in the region of the pK values. The 2JCH, 3JCH, and 3JHH couplings needed for spin order transfer vary with pH and are best resolved at low pH leading to our use of pH approximately 3 for both the molecular addition of parahydrogen to 1-13C-fumaric acid-d2 and the subsequent transfer of spin order from the nascent protons to C1 of the succinic acid product. The methods described here may generalize to hyperpolarization of other carboxylic acids. The C1 spin-lattice relaxation time at neutral pH and 4.7 T is measured as 27 s in H2O and 56 s in D2O. Together with known rates of succinate uptake in kidneys, this allows an estimate of the prospects for the molecular spectroscopy of metabolism. Published 26 March 2008 in J Am Chem Soc, 130(13): 4212-3. Articles on NMR published 20 December 2007: Effect of the magnetic field on the supramolecular structure of chiral smectic C phases: (2)H NMR studies. Chemphyschem, 8(18): 2575-87. We present a theoretical and experimental (2)H NMR study of the effect of external magnetic fields on the supramolecular organization of chiral smectic liquid-crystalline mesophases, such as SmC* and re-entrant SmC*. Three experimental cases in which the supramolecular helical structure of the smectic C* phase is unwound by a magnetic field (H), parallel to the helical axes of this phase, are discussed in detail. Unwinding of the helical structure is described by using a theoretical model based ... [Abstract] [Full-text] Articles on NMR published 25 October 2007: The binding affinities of a selected series of Gd(III) chelates bearing bile acid residues, potential hepatospecific MRI contrast agents, to a liver cytosolic bile acid transporter, have been determined through relaxivity measurements. The Ln(III) complexes of compound 1 were selected for further NMR structural analysis aimed at assessing the molecular determinants of binding. A number of NMR experiments have been carried out on the bile acid-like adduct, using both diamagnetic Y(III) and ... [Abstract] [Full-text] Articles on NMR published 22 October 2007: Purity analysis of hydrogen cyanide, cyanogen chloride and phosgene by quantitative (13)C NMR spectroscopy. Magn Reson Chem, 45(11): 954-61. Hydrogen cyanide, cyanogen chloride and phosgene are produced in tremendously large quantities today by the chemical industry. The compounds are also particularly attractive to foreign states and terrorists seeking an inexpensive mass-destruction capability. Along with contemporary warfare agents, therefore, the US Army evaluates protective equipment used by warfighters and domestic emergency responders against the compounds, and requires their certification at > or = 95 carbon atom % before ... [Abstract] [Full-text] Articles on NMR published 26 September 2007: Principal component analysis of the pH-dependent conformational transitions of bovine beta-lactoglobulin monitored by heteronuclear NMR. Proc Natl Acad Sci U S A, 104(39): 15346-51. To clarify the pH-dependent conformational transitions of proteins, we propose an approach in which structural changes monitored by heteronuclear sequential quantum correlation (HSQC) spectroscopy were analyzed by using a principal component analysis (PCA). We use bovine beta-lactoglobulin, a protein widely used in protein folding studies, as a target. First, we measured HSQC spectra at various pH values and subjected them to a PCA. The analysis revealed three apparent transitions with pK(a) ... [Abstract] [Full-text] Articles on NMR published 25 September 2007: Structural biology of transmembrane domains: efficient production and characterization of transmembrane peptides by NMR. Protein Sci, 16(10): 2153-65. Structural characterization of transmembrane peptides (TMPs) is justified because transmembrane domains of membrane proteins appear to often function independently of the rest of the protein. However, the challenge in obtaining milligrams of isotopically labeled TMPs to study these highly hydrophobic peptides by nuclear magnetic resonance (NMR) is significant. In the present work, a protocol is developed to produce, isotopically label, and purify TMPs in high yield as well as to initially ... [Abstract] [Full-text] Articles on NMR published 21 September 2007: 13C-13C NMR spin-spin coupling constants in saccharides: structural correlations involving all carbons in aldohexopyranosyl rings. J Org Chem, 72(20): 7511-22. 13C-13C Spin-spin coupling constants (JCC) have been measured in a group of aldohexopyranoses and methyl aldopyranosides singly labeled with 13C at different sites to confirm and extend prior correlations between JCC magnitude and sign and saccharide structure. Structural correlations for 2JC1,C3, 2JC2,C4, 2JC4,C6, and 2JC1,C5 have been confirmed using density functional theory calculations to test empirical predictions. These geminal couplings depend highly on the orientation of C-O bonds ... [Abstract] [Full-text] Articles on NMR published 20 September 2007: NMR-spectroscopy-based metabonomic approach to the analysis of Bay41-4109, a novel anti-HBV compound, induced hepatotoxicity in rats. Toxicol Lett, 173(3): 161-7. An integrated metabonomics study using high-resolution (1)H nuclear magnetic resonance (NMR) spectroscopy has been applied to investigate the biochemical composition of urine, serum, liver tissue aqueous extracts (acetonitrile/water) and liver tissue lipidic extracts (chloroform/methanol) obtained from control and Bay41-4109 treated rats (10, 50, 400mg.kg(-1).d(-1) for 5 days, i.g.). Principal components analysis was used to visualize similarities and differences in biochemical profiles. The ... [Abstract] [Full-text] Quantitative analysis of liver metabolites in three stages of the circannual hibernation cycle in 13-lined ground squirrels by NMR. Physiol Genomics, 31(1): 15-24. Thirteen-lined ground squirrels and other circannual hibernators undergo profound physiological changes on an annual basis, transitioning from summer homeothermy [body temperature (T(b)) approximately 37 degrees C] to winter heterothermy (T(b) cycling between 0 degrees C and 37 degrees C). We hypothesize that these physiological changes are reflected in biochemical changes that provide mechanistic insights into, and biomarkers for, hibernation states. Here we report the results of an NMR-based ... [Abstract] [Full-text] © 2005-2008 NMR Research Today. All Rights Reserved. |
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