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  • Analytical Chemistry and Spectroscopy  (2)
  • Antamanide  (1)
  • 2020-2024
  • 1995-1999  (3)
  • 1
    ISSN: 1573-5001
    Keywords: 2D heteronuclear NMR ; Isotope labeling ; Coupling constants ; Antamanide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Summary A simple heteronuclear relayed E.COSY pulse sequence with a minimum number of pulses is proposed for the quantitative determination of heteronuclear three-bond J-coupling constants in uniformly 13C-enriched polypeptide samples. Numerous heteronuclear three-bond coupling constants, including $${}^3{\text{J}}_{{\text{H}}^{\text{N}} {\text{C}}'} $$ , $${}^3{\text{J}}_{{\text{H}}^{\text{N}} {\text{C}}^\beta } $$ , $${}^3{\text{J}}_{{\text{H}}^\beta {\text{C}}'} $$ , and $${}^3{\text{J}}_{{\text{H}}^\alpha {\text{C}}^\gamma } $$ , can be determined for each residue from a single heteronuclear relayed E.COSY spectrum. Couplings relevant for stereospecific assignments as well as for the determination of dihedral angles in the amino acid backbone and in side chains are obtained. The method is demonstrated on the uniformly 13C-enriched decapeptide antamanide (-Val1-Pro2-Pro3-Ala4-Phe5-Phe6-Pro7-Pro8-Phe9-Phe10-).
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The electron impact mass spectra of nine solanidane N-oxides show, in addition to the known typical fragmentation pattern of the solanidane moiety, the fragment ions [M - C5H9]+ and [C6H12NO]+, due to thermal Cope syn-eliminations caused by the N-oxide function and subsequent cleavage of the bonds between C(22) and C(23) and between C(20) and C(22), respectively, in the so-obtained cyclic N,N-dialkylhydroxylamines.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 30 (1995), S. 1489-1494 
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The glucosyl ester (2b), the galactosyl ester (3b), the xylosyl ester (4b) and the arabinosyl ester (5b) of gibberellin A3 (GA3) as well as the glucosyl ester (7b) and the xylosyl ester (8b) of isoGA3 were synthesized and their structures confirmed especially by 1H nuclear magnetic resonance. In order to identify such conjugates in nature, the glycosyl esters 2b, 3b, 4b, 5b, 7b and 8b were subjected to mass spectrometry analysis using fast atom bombardment and electrospray ionization techniques. The spectra obtained from both negative and positive ions were compared and interpreted on the basis of tandem mass spectrometry experiments. The differences between the fragmentation of GA3 glycosyl ester and that of isoGA3 glucosyl ester are discussed. Diagnostic ions were evaluated, which should be useful for the identification of these conjugates by liquid chromatography/mass spectrometry.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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