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  • 1
    Electronic Resource
    Electronic Resource
    Mass spectrometric fragmentation patterns for the Syn and Anti isomers of PGE2 and PGD2- methyloxime methyl esters and their analogs (1985)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1985), S. 303-308 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A systematic study of the mass spectral fragmentation of the methyl ester-methyloxime-trimethylsilyl ether derivatives of D and E prostaglandins and selected ω-chain analogs is presented. Fragments from the ω-chain analogs are shifted the appropriate mass when compared with the parent PGD2 or PGE2. NMR data of the methyloxime methyl ester of PGE2 have permitted assignment of the syn and anti isomers (relative to the α chain) to the fast and slow eluting gas chromatographic peaks, respectively.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200120702
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    Small molecule conformation in the receptor-bound state by the two-dimensional spin exchange experiment (1987)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 25 (1987), S. 1025-1034 
    Details
    ISSN: 0749-1581
    Keywords: Nuclear Overhauser effect ; Potein-ligand interaction ; Spin diffusion Prostaglandin ; 2α ; Bound state conformation ; Time saving strategy ; t1 streak subtraction ; NOESY NAD+ ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pure absorption phase two-dimensional nuclear Overhauser spectrocopy (NOESY), using a short cycle time protocol, has been used to study cross-relaxation between protons of ligands bound to proteins. The 2D experiment is an accurate and efficient method for determining exchange transferred NOEs. Truncated NOESY data sets (obtained in less than 3 h) for the test systems - prostaglandin F2α bound to albumin and NAD+ bound to three different dehydrogenase enzymes - provide NOE estimates within experimental error of those obtained by the more time-consuming one-dimensional experiments. The 2D data matrix has within it spin-diffusion controls and cross-relaxation spectra useful for the subtraction of unwanted signals including spin transfer from coincidentally perturbed protein resonances and t1 streaks and ridges.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260251202
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    Paper (German National Licenses)
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  • 3
    Electronic Resource
    Electronic Resource
    Quantitative small molecule NOESY. A practical guide for derivation of cross-relaxation rates and internuclear distances (1989)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 27 (1989), S. 515-528 
    Details
    ISSN: 0749-1581
    Keywords: NOESY quantitation ; Short repetition times ; Incomplete recovery ; Small molecule cross-relaxation rates ; Conformational analysis ; Secondary NOEs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The pure absorption 2D NOE experiment can provide small molecule cross-relaxation rate data suitable for quantitative conformational analysis even when the data are collected in a time-saving manner using preparatory delays (PD) far short of the recommended values of 3-5 times T1. In our experience, the relative NOE intensities and cross-relaxation rates are most readily extracted from cross-relaxation spectra which are sums of adjacent rows (or columns) of the 2D data matrix. Intensity anomalies associated with t1 streaks can be removed by plotting cross-relaxation difference spectra. PD truncation produces significant deviations from diagonal symmetry which must be accounted for in the data analysis. The influence of PD truncation on apparent auto-peak decay rates and cross-/auto-peak intensity ratios is examined in both real and simulated spectra in order to develop appropriate quantitation strategies. These strategies, when applied to NOESY data for aqueous prostaglandin (PG) F2 α and a PG analog in organic media, yield cross-relaxation rates that are within experimental error of those calculated from structural models or determined by more time-consuming 1D NOE methods.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260270603
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    Paper (German National Licenses)
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