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Signal Assignments (signal + assignment)
Kinds of Signal Assignments Selected AbstractsHIGH-RESOLUTION MAGIC ANGLE SPINNING NMR ANALYSIS OF WHOLE CELLS OF CHAETOCEROS MUELLERI (BACILLARIOPHYCEAE) AND COMPARISON WITH 13C-NMR AND DISTORTIONLESS ENHANCEMENT BY POLARIZATION TRANSFER 13C-NMR ANALYSIS OF LIPOPHILIC EXTRACTS,JOURNAL OF PHYCOLOGY, Issue 3 2004Matilde S. Chauton Lipid composition in extracted samples of Chaetoceros muelleri Lemmermann was studied with 13C-NMR and distortionless enhancement by polarization transfer (DEPT) 13C-NMR, resulting in well-resolved 13C-NMR spectra with characteristic resonance signals from carboxylic, olefinic, glyceryl, methylene, and methyl groups. The application of a DEPT pulse sequence aided in the assignment of methylene and methine groups. Resonance signals were compared with literature references, and signal assignment included important unsaturated fatty acids such as eicosapentaenoic and docosahexaenoic and also phospholipids and glycerols. Results from the extracted samples were used to assign resonance signals in a high-resolution magic angle spinning (HR MAS) DEPT 13C spectrum from whole cells of C. muelleri. The NMR analysis on whole cells yielded equally good information on fatty acids and also revealed signals from carbohydrates and amino acids. Broad resonance signals and peak overlapping can be a problem in whole cell analysis, but we found that application of HR MAS gave a well-resolved spectrum. The chemical shift of metabolites in an NMR spectrum depends on the actual environment of nuclei during analysis, and some differences could therefore be expected between extracted and whole cell samples. The shift differences were small, and assignment from analysis of lipophilic extract could be used to identify peaks in the whole cell spectrum. HR MAS 13C-NMR therefore offers a possibility for broad-range metabolic profiling directly on whole cells, simultaneously detecting metabolites that are otherwise not detected in the same analytical set up and avoiding tedious extraction procedures. [source] A new technique for differentiating between 2J(C,H) and 3/4J(C,H) connectivitiesMAGNETIC RESONANCE IN CHEMISTRY, Issue 3 2003Thomas Sprang Abstract We present a new pulse sequence that yields two simultaneously detected types of long-range correlation spectra. The one spectrum is to show all nJ(C,H) connectivities and the other is to show exclusively 2J(C,H) connectivities. The method is demonstrated by using strychnine as a test sample. A comparison with HMBC shows that the 2J(C,H)/nJ(C,H) experiment supplies a nJ(C,H) spectrum that is of equal standard with regard to sensitivity and spectral information. The additional 2J(C,H) spectrum allows the disentanglement of 2J(C,H) and nJ(C,H) signals (n > 2) in HMBC type spectra, which greatly simplifies signal assignment and structure elucidation in general. Copyright © 2003 John Wiley & Sons, Ltd. [source] DFT-GIAO1H NMR chemical shifts prediction for the spectral assignment and conformational analysis of the anticholinergic drugs (,)-scopolamine and (,)-hyoscyamineMAGNETIC RESONANCE IN CHEMISTRY, Issue 6 2010Marcelo A. Muñoz Abstract The relatively large chemical shift differences observed in the 1H NMR spectra of the anticholinergic drugs (,)-scopolamine 1 and (,)-hyoscyamine 2 measured in CDCl3 are explained using a combination of systematic/molecular mechanics force field (MMFF) conformational searches and gas-phase density functional theory (DFT) single point calculations, geometry optimizations and chemical shift calculations within the gauge including/invariant atomic orbital (GIAO) approximation. These calculations show that both molecules prefer a compact conformation in which the phenyl ring of the tropic ester is positioned under the tropane bicycle, clearly suggesting that the chemical shift differences are produced by the anisotropic effect of the aromatic ring. As the calculations fairly well predict these experimental differences, diastereotopic NMR signal assignments for the two studied molecules are proposed. In addition, a cursory inspection of the published 1H and 13C NMR spectra of different forms of 1 and 2 in solution reveals that most of them show these diastereotopic chemical shift differences, strongly suggesting a preference for the compact conformation quite independent of the organic or aqueous nature of the solvent. Copyright © 2010 John Wiley & Sons, Ltd. [source] 13C and 1H NMR signal assignments of some new synthetic dehydroabietic acid derivativesMAGNETIC RESONANCE IN CHEMISTRY, Issue 4 2008Marinaldo S. de Carvalho Abstract The 1H and 13C NMR signal assignments of a series of new synthetic derivatives of dehydroabietic acid are presented. Copyright © 2008 John Wiley & Sons, Ltd. [source] 1H and 13C NMR signal assignments of Paecilin A and B, two new chromone derivatives from mangrove endophytic fungus Paecilomyces sp. (tree 1,7)MAGNETIC RESONANCE IN CHEMISTRY, Issue 9 2007Zhiyong Guo Abstract Two new natural products, named paecilin A (1) and B (2), together with two known compounds secalonic acid D (3) and (11)-cytochalasa-6(12),13-diene-1,21-dione-16,18-dimethyl-7-hydroxy-l0-phenyl-(7S*,13E,16S*,18S*) (4), were isolated from the mangrove endophytic fungus, Paecilomyces sp. (tree 1,7) from the South China Sea. 1D and 2D NMR experiments including COSY, HMQC, and HMBC were used for the determination of their structures. In our cytotoxicity assays, secalonic D (3) showed cytotoxicity toward KB cells with IC50 < 1 µg ml,1 and inhibiting human topoisomerase I with IC50 at 0.16 µmol ml,1. 1, 2, and 4 showed no activity to KB cells. Copyright © 2007 John Wiley & Sons, Ltd. [source] Complete NMR signal assignments of flavonol derivativesMAGNETIC RESONANCE IN CHEMISTRY, Issue 2 2006Hojung Kim Abstract Common substitution positions of flavonols are at C-5 and C-7; 6-substituted flavonol derivatives are rarely found in natural sources. Here, we report complete assignments of 1H and 13C chemical shifts of eight flavonol derivatives including four 6-substituted flavonols. Copyright © 2005 John Wiley & Sons, Ltd. [source] NMR study on 9- S and 9- R oxirane derivatives of ascomycinMAGNETIC RESONANCE IN CHEMISTRY, Issue 7 2002K. Baumann Abstract Structure elucidation of 9- S and 9- R oxirane derivatives of ascomycin, a 23-membered immunomodulating macrolactam, was performed using NMR spectroscopy. The total 1H and 13C signal assignments required the gradient-selected versions of COSY (gs-COSY), heteronuclear multiple quantum-correlation spectroscopy (gs-HSQC), heteronuclear multiple-bond correlation spectroscopy (gs-HMBC), and nuclear Overhauser methods. The data sets then were used to examine the dependence of ketone,hemiketal and cis,trans amide equilibria on the substitution pattern and the absolute configuration of the chiral oxirane. Copyright © 2002 John Wiley & Sons, Ltd. [source] Hexamer oligonucleotide topology and assembly under solution phase NMR and theoretical modeling scrutinyBIOPOLYMERS, Issue 12 2010Maxim P. Evstigneev Abstract The entire family of noncomplementary hexamer oligodeoxyribonucleotides d(GCXYGC) (X and Y = A, G, C, or T) were assessed for topological indicators and equilibrium thermodynamics using a priori molecular modeling and solution phase NMR spectroscopy. Feasible modeled hairpin structures formed a basis from which solution structure and equilibria for each oligonucleotide were considered. 1H and 31P variable temperature-dependent (VT) and concentration-dependent NMR data, NMR signal assignments, and diffusion parameters led to d(GCGAGC) and d(GCGGGC) being understood as exceptions within the family in terms of self-association and topological character. A mean diffusion coefficient D298 K = (2.0 ± 0.07) × 10,10 m2 s,1 was evaluated across all hexamers except for d(GCGAGC) (D298 K = 1.7 × 10,10 m2 s,1) and d(GCGGGC) (D298 K = 1.2 × 10,10 m2 s,1). Melting under VT analysis (Tm = 323 K) combined with supporting NMR evidence confirmed d(GCGAGC) as the shortest tandem sheared GA mismatched duplex. Diffusion measurements were used to conclude that d(GCGGGC) preferentially exists as the shortest stable quadruplex structure. Thermodynamic analysis of all data led to the assertion that, with the exception of XY = GA and GG, the remaining noncomplementary oligonucleotides adopt equilibria between monomer and duplex, contributed largely by monomer random-coil forms. Contrastingly, d(GCGAGC) showed preference for tandem sheared GA mismatch duplex formation with an association constant K = 3.9 × 105M,1. No direct evidence was acquired for hairpin formation in any instance although its potential existence is considered possible for d(GCGAGC) on the basis of molecular modeling studies. © 2010 Wiley Periodicals, Inc. Biopolymers 93: 1023,1038, 2010. This article was originally published online as an accepted preprint. The "Published Online" date corresponds to the preprint version. You can request a copy of the preprint by emailing the Biopolymers editorial office at biopolymers@wiley.com [source] | ||||||||||