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  • Analytical Chemistry and Spectroscopy  (133)
  • Biochemistry and Biotechnology  (63)
  • EARTH RESOURCES AND REMOTE SENSING
  • INSTRUMENTATION AND PHOTOGRAPHY
  • 1995-1999  (220)
  • 1980-1984
  • 1995  (220)
Collection
Keywords
Publisher
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  • 1995-1999  (220)
  • 1980-1984
Year
  • 11
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Tandem mass spectrometric methods for the identification of 19-nortestosterone (estr-4-en-17β-3-one) are described and evaluated. The fragmentation reactions of the heptafluorobutyryl (HFB) and pentafluorobenzyloxime heptafluorobutyryl (PFBO—HFB) ester derivatives of 19-nortestosterone in particular were studied for the purpose to select characteristic ions. The HFB ester was analyzed by collisionly activated dissociation (CAD) following electron impact in order to fragment the steroid nucleus. Cleavage of the A-ring, i.e. the ring containing the keto function, was prominent. The formation of A-, A/B- and D-ring fragments was also typical for this type of derivative. The PFBO—HFB ester was formed to create a derivative, which could capture electrons and be analyzed in the electron-capture negative chemical ionization (ECNCI) mode. Besides fragmentations originating in the groups coupled to the steroid by derivatization, no prominent steroid nucleus fragmentations were observed by CAD following ECNCI. Accordingly, of both methods only CAD following EI of the HFB derivative of 19-nortestosterone provided a characteristic MS/MS procedure for the identification of 19-nortestosterone.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 12
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 9 (1995), S. 114-118 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Dissociation of C60- ions induced in 30 keV collisions with atomic and molecular gases has been studied. The pattern of negativeion formation from C60- precursors is found to be distinctly different from that obtained for positive-ion fragments from C60+ precursors in that the collision-induced dissociation spectrum in the former case is dominated by small negative clusters, presumably of linear geometry, Simple arguments utilizing the relationship of electrostatic properties of different molecular structures to their electron affinities and ionization energies have been invoked to rationalize these observations. The difference in the dissociation dynamics of C60- and C60+ ions is discussed in terms of competition between different energy-coupling schemes involving either electronic degrees of freedom or nuclear (vibrational) degrees of freedom.
    Additional Material: 4 Ill.
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  • 13
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 9 (1995), S. 1376-1379 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The mass spectrometric behaviour of two pairs of fluorinated vinyl- and allyl-ethers and thioethers has been studied in detail with the aid of metastable ion data and accurate mass measurements. Clear differences have been observed between the two sets of compounds; while for the ethers the McLafferty rearrangement with ethylene loss represents a highly favoured decomposition route, for the thioethers the loss of the ethyl radical is preferred. Some decomposition routes, common to all the compounds examined, suggest the presence of hydrogen atom bridging between carbon and fluorine atoms. Theoretical calculations have shown that such a quasi C—H—F structure is already present in the neutral molecule in its ground state.
    Additional Material: 3 Ill.
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  • 14
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The electron-ionization induced mass spectra of some N-monosubstituted fluoroacetamides of the general formula FCH2—CONH—R, in which the substituent R is (C3—C7) cycloalkyl, phenyl, 4-methylphenyl, 4-carbo-methoxyphenyl, 4-nitrophenyl and 4-diethylaminophenyl, were recorded and their fragmentation patterns were studied by metastable-ion analyses.
    Additional Material: 2 Tab.
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  • 15
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A mass fragmentographic method for the measurement in plasma of underivatized, dehydrated 25-hydroxyvitamin D2 and 25-hydroxyvitamin D3 was developed. Quantitative dehydration of vitamin D metabolites was achieved prior to gas chromatography using a new high-temperature injection system and a small precolumn packed with aluminium powder in the injection port, followed by mass fragmentography on an inexpensive bench-top mass spectrometer. Plasma (2 ml) was incubated with hexadeuteriated 25-hydroxyvitamin D3 prior to acetonitrile extraction and purification using cartridges pre-packed with microparticulate silica using reversed- and normal-phase solvent systems. After purification, capillary gas chromatography mass spectrometry was carried out following dehydration of the secosteroids on the aluminium power pre-column at 400°C. High-intensity dehydrated molecular ions were produced which were used for selected ion monitoring. The assay sensitivity for 25-hydroxyvitamin D was approximately 1 ng ml-1. The intra-assay variation was less than 7% and the recovery of added standard was quantitative. It is suggested that this method may be used to provide target values for much needed quality control schemes to monitor assays routinely used in the estimation of 25-hydroxyvitamin D. The behaviour of a number of other hydroxylated vitamin D metabolites, when injected without derivatization on to a gas chromatographic column, was also investigated.
    Additional Material: 10 Ill.
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  • 16
    ISSN: 0749-1581
    Keywords: NMR ; 1H NMR spectroscopy ; photocycloaddition ; meta photocycloadducts ; 4-phenoxybut-1-enes ; 3-benzyloxyprop-1-enes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1H NMR data (400 and 500 MHz) are reported for the intramolecular meta photocycloaddition products from 4-phenoxybut-1-enes and 3-benzyloxyprop-1-enes. The structures of these photoproducts, and in particular the discrimination between the 1,6- and 7,8-bridged isomers, are deduced from COSY 45 and 60 experiments and spin-decoupling techniques.
    Additional Material: 5 Tab.
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  • 17
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 33 (1995), S. 497-499 
    ISSN: 0749-1581
    Keywords: NMR ; 1H NMR ; 13C NMR ; 6-s-trans-retinoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new class of vitamin A analogs (retinoids) was synthesized containing a dimethylene bridge to maintain a 6-s-trans conformation of the terminal double bonds. The 1H and 13C NMR spectra were assigned for 15 new compounds, including E-Z isomers (all-E, 13Z, 9Z and 9Z,13Z) of retinoids containing an ethyl ester and car-boxylic acid polar end groups, and also the (all-E)-isomer of the retinoids with an alcohol and aldehyde polar end-groups and five C15 intermediates. The assignments were based on long-range 1H—13C heteronuclear 2D experiments.
    Additional Material: 1 Ill.
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  • 18
    ISSN: 0173-0835
    Keywords: Capillary electrophoresis ; Experimental design ; Optimisation ; Robustness ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Various chemometric experimental designs have been employed for the optimisation of capillary electrophoresis (CE) methods. Similar designs have been utilised in the assessment of the robustness of CE methods. The designs employed include central composites, fractional factorials, Plackett-Burman, simplex and overlapping-resolution mapping. Optimisation studies have largely concentrated on the use of these designs on selection of the optimal electrolyte composition. The robustness testing studies performed have involved the use of screening designs to identify the critical parameters affecting responses such as migration times and resolution. Further designs such as central composites have then been employed to set method limits following robustness studies. It is concluded that the use of experimental designs and statistical data evaluation in conjunction with personal computer-controlled CE autosamplers and instruments are of great benefit in the optimisation and robustness evaluation of CE methods.
    Additional Material: 6 Ill.
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  • 19
    Electronic Resource
    Electronic Resource
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 26 (1995), S. 911-916 
    ISSN: 0377-0486
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Fourier transform (FT) Raman spectra of the cell walls of three species of fungi are reported for the first time, namely (i) Agaricus bisporus, a fruiting bud, (ii) Mortierella genus and (iii) Mucor genus. Some molecular assignments are proposed for the major vibrational features and attributed to chitin, N-acetylglucosamine and (R)-glucan. Preliminary studies indicate that it is possible to use FT-Raman spectroscopy to discriminate between different mixed species in culture media.
    Additional Material: 4 Ill.
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  • 20
    Electronic Resource
    Electronic Resource
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 26 (1995), S. 1039-1043 
    ISSN: 0377-0486
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A constrained non-linear deconvolution method was used to analyse the Raman spectrum of amorphous carbon. The method was tested by applying it to a model spectrum. Before the deconvolution the observed Raman spectrum was smoothed by a least-squares convoluting procedure. The proper width of the spread function used in the deconvolution was determined by examining the reversibility of the deconvolution process. The deconvolution result for the Raman spectrum of amorphous carbon has a form very similar to the phonon density of states of graphite. This is taken to be additional evidence for Shuker and Gamon's model for Raman spectra of amorphous materials. Potentially, the deconvolution method can also be used for other aspects of Raman spectrum analysis of amorphous materials, such as finding the relative intensity of each peak of study the structure of the material.
    Additional Material: 4 Ill.
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