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  • Articles  (10)
  • Analytical Chemistry and Spectroscopy  (10)
  • 2020-2021
  • 1990-1994  (5)
  • 1985-1989  (5)
  • 1950-1954
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  • Articles  (10)
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  • 1
    Electronic Resource
    Electronic Resource
    Characterization of glutathione conjugates by fast atom bombardment/tandem mass spectrometry (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 615-621 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The collisionally activated decomposition of [M + H]+ ions, generated by fast atom bombardment (FAB) of glutathione conjugates, has been studied by tandem mass spectrometry (MS/MS) using hybrid sector/quadrupole instruments. Abundant fragments of diagnostic utility were present in the daughter ion spectra. Common fragmentation modes were observed but their relative importance was strongly dependent on the nature of the conjugated species. As an example of a general approach to the characterization of glutathione conjugates in biological samples, the acetaminophen-glutathione conjugate was identified in rat bile, following coadministration of (2H0)- and (2H3)acetaminophen, using the experimental sequence: (i) conventional FAB mass spectrometric analysis, (ii) MS/MS using constant neutral loss (129 u) scanning to identify parent ions corresponding to glutathione conjugates, (iii) MS/MS to yield daughter ion spectra of parents so identified and corresponding to (2H0)- and (2H3)-labeled conjugates.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200151107
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  • 2
    Electronic Resource
    Electronic Resource
    Molecular fragmentation patterns of carbon dioxide at very high internal energies (1993)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 28 (1993), S. 340-343 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ion-ion coincidence measurements following K-shell absorption in the carbon dioxide molecule were performed by applying time-of-flight mass spectrometry in conjunction with monochromatic synchrotron radiation and electron impact. Identification of particularly sensitive electronic transitions and the consecutive molecular fragmentation in real time was performed. Analysis of coincidence recordings from decomposition of carbon dioxide reveals one distinct pathway in which three cations are formed following excitation of oxygen Is electrons.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210280413
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  • 3
    Electronic Resource
    Electronic Resource
    Fast-atom bombardment/mass-analysed ion kinetic energy spectrometry of inositol phosphates (1993)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 7 (1993), S. 555-560 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The application of fast-atom bombardment mass Spectrometry and collisiorutlly induced dissociation with mass-analysed ion kinetic energy (CID/MIKE) Spectrometry of representative inositol mono-, bis- and trisphos-phates is described. Based on their CID/MIKE spectra, inositol polyphosphates containing vicinal phosphate groups could be distinguished from isomers in which adjacent phosphate groups were absent. The potential value of this procedure in studies of the biochemistry of intracellular second messengers is discussed.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290070631
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  • 4
    Electronic Resource
    Electronic Resource
    Selected reaction monitoring during gas chromatography/mass spectrometry of eicosanoids (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1988), S. 409-413 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatography/electron capture negative ion mass spectrometry of eicosanoids, as pentafluorobenzyl (PFB) ester, methyl oxime (where applicable), trimethylsilyl (TMS) ether derivatives, is reported using a double-focusing instrument of trisector configuration. Sub-picogram detection limits were observed for prostaglandins E1, E2 and F2α during selected ion monitoring (SIM) of [M — PFB]- ions. Selected reaction monitoring (SRM) of [M — PFB]- → [M — PFB — TMSOH]-, occurring in the first field-free region, was of modest sensitivity, reflecting the stability of the [M - PFB]- ions. The leukotriene B4 (LTB4) derivative was successfully analyzed by SIM at the low-picogram level. In this instance, the fragmentation [M — PFB]- →[M — PFB — TMSOH] occurred in high yield in the first field-free region. The advantageous improvement in selectivity of detection that may be achieved with SRM was evident during the analysis of a serum extract for LTB4.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200160180
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  • 5
    Electronic Resource
    Electronic Resource
    Characterization of glucuronic acid conjugates of a novel angiotensin receptor antagonist (1994)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 8 (1994), S. 217-221 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Nanogram quantities of glucuronic acid conjugates of GR117289 in rat and dog bile have been analysed by semi-microbore high-performance liquid chromatography (HPLC)/ionspray mass spectrometry with on-line UV diode array detection. The determination of drug metabolites in bile has often proved problematical due to the large number of endogenous components in this biological matrix, in particular the bile acids. Semi-microbore HPLC is useful for concentrating small quantities of material and, in combination with an on-line diode array detector, for distinguishing between drug related and endogenous components. A novel angiotensin II receptor antagonist, GR117289, had proved difficult to analyse by thermospray mass spectrometry because of its thermal lability. The use of the less thermally dependent technique of ionspray mass spectrometry allowed the characterization of nanogram quantities of glucuronic acid metabolites of GR117289 in bile.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290080218
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  • 6
    Electronic Resource
    Electronic Resource
    Application of relayed coherence transfer two-dimensional nuclear magnetic resonance spectroscopy to the assignment of 1H chemical shifts in steroids (1988)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 26 (1988), S. 214-223 
    Details
    ISSN: 0749-1581
    Keywords: RELAY 2D NMR ; 1H NMR ; 2D NMR Steroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Relayed coherence transfer (RELAY) two-dimensional NMR spectroscopy was demonstrated to be an effective technique for overcoming the problem of overlapping multiplets in the analysis of the 1H NMR spectra of steroids. Cross-sections through appropriate proton resonances resulted in resolved spectra of the spin systems for each of the saturated rings of the estrogenic hormones 17β- and 17α-estradiol. During RELAY experiments with a fixed delay time of 0.042 s it was possible to observe RELAY cross-peaks between H-11α and 18-CH3 which resulted from magnetization transfer via long-range coupling between 18-CH3 and H-12α. The difference in stereochemistry at C-17 of these estradiol epimers allowed an examination of the effect of substituent configuration on the RELAY cross-peak intensity in order to determine the ability of the RELAY method to provide qualitative structural information.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260260308
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  • 7
    Electronic Resource
    Electronic Resource
    Structures of zearalenone and zearalanone in solution: A high-field NMR and molecular modelling study (1990)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 28 (1990), S. 835-845 
    Details
    ISSN: 0749-1581
    Keywords: Zearalenone ; Zearalanone ; 1H and 13C NMR ; Molecular modelling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The complete 1H and 13C NMR spectra of the mycotoxin zearalenone are described. An analysis of all the vicinal proton-proton coupling constants, together with molecular modelling results, leads to a three-dimensional structure very similar to those observed x-ray crystallographically for related systems. Analogous data on zearalanone reveal that whereas the overall molecular geometry is similar to that of zearalenone, the alkyl terminus of the 12-membered bridging moiety is now oriented almost orthogonally to the aromatic ring plane.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260281002
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  • 8
    Electronic Resource
    Electronic Resource
    NMR of the methylene group: Artifacts in the proton-proton decoupled heteronuclear two-dimensional chemical shift correlation experiment (1988)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 26 (1988), S. 1058-1061 
    Details
    ISSN: 0749-1581
    Keywords: Two-dimensional NMR ; Artifacts ; BIRD pulses ; Coherence transfer ; Methylene groups ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: When the proton-proton decoupled heteronuclear two-dimensional chemical shift correlation experiment is applied to a molecule containing methylene groups, the spectra show not only the expected signals at the two proton chemical shifts, but also a strong artifact. This artifact appears at the average of the two proton chemical shifts, and arises from coherence transfer between the two protons caused by the BIRD pulse. It is not caused by strong coupling between the protons, and so may appear in any spectrum. The dependence of this artifact on experimental conditions was analysed, and is illustrated with results obtained on the methylene groups from the cyclophane ring in N6′,N9-octamethylenepurinecyclophane.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260261205
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  • 9
    Electronic Resource
    Electronic Resource
    NMR analysis of fluorinated corticosteroids related to fluocinonide: Detection of long-range 1H-19F couplings using the heteronuclear equivalent of the COSY experiment (1991)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 29 (1991), S. 387-397 
    Details
    ISSN: 0749-1581
    Keywords: 1H NMR ; 19F Corticosteroids ; 1H-19F long-range coupling ; Heteronuclear COSY ; 1H-19F 2D correlation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of the 1H and 19F NMR spectra of the corticosteroid fluocinonide and five related steroids is reported. The 500 MHz 1H NMR spectra revealed several previously undetected long-range 1H-19F coupling constants. These couplings were assigned by the application of the heteronuclear equivalent of the COSY pulse sequence. The fluorine substituent effects and long-range heteronuclear couplings were examined in relation to structures derived from molecular mechanics (MMX) calculations.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260290417
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  • 10
    Electronic Resource
    Electronic Resource
    Identification of C-glycopyranosides and C-glycofuranosides by 13C NMR and 1H NMR. Complete assignment of their spectral data using carbon-proton chemical shift correlation spectroscopy (1988)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 26 (1988), S. 1062-1067 
    Details
    ISSN: 0749-1581
    Keywords: 1H ; 13C NMR 2D NMR ; C-Glycopyranosides ; C-Glycofuranosides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: C-Glycopyranosides and C-glycofuranosides were identified using 13C and 1H chemical shift and coupling constant data. Full assignments for all α- and β-anomers were made possible by recourse to carbon-proton chemical shift correlation spectroscopy. Greater steric shielding effects were observed on the carbon atoms in cis-1,2-substituted compounds compared with their trans counterparts. Consistent proton chemical shift differences were also noted in that the anomeric protons resonate at lower field in all cis-1,2-isomers.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260261206
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