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  • Analytical Chemistry and Spectroscopy  (863)
  • EARTH RESOURCES AND REMOTE SENSING  (560)
  • 2010-2014
  • 1980-1984  (1,423)
  • 1925-1929
  • 1984  (1,423)
Collection
Keywords
Publisher
Years
  • 2010-2014
  • 1980-1984  (1,423)
  • 1925-1929
Year
  • 201
    Electronic Resource
    Electronic Resource
    Theoretical derivation of fluorescent x-ray intensities in x-ray fluorescence spectrochemical analysis (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 52-54 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The theoretical equations for primary, secondary and tertiary fluorescent x-ray intensities have been given by Shiraiwa and Fujino. However, their derivation is unsatisfactory in some respects. In this paper these problems are discussed and a more correct derivation is given.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130203
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  • 202
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    Masthead (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984) 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130101
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  • 203
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    Consideration of an enhancement effect simplified expression in limiting cases in x-ray fluorescence analysis (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 23-26 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The problem of a simplified expression for the enhancement term of correction equations in XRF analysis was treated using the example of binaries. Attention was paid to up-to-date propositions of a solution to that problem and new cases of solutions were considered. Some common elements of these solutions were found and on the basis of a fundamental expression of enhancement effects a more general equation is given.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130105
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  • 204
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    Energy-dispersive x-ray fluorescence analysis of silicate rocks for major and trace elementsAn earlier version of this paper was presented at the 12th X-Ray Spectrometry Conference, Durham, England, September 1980. (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 2-15 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The performance of an energy-dispersive x-ray fluorescence (ED-XRF) system for the analysis of silicate rocks was investigated in detail. Data are presented to demonstrate the selection of optimum excitation conditions for the major elements (Na-Fe), analysed on glass beads, and the trace elements (particularly the Rb-Nb group) analysed on powder pellets. Limitations in spectrum analysis due to overlap interferences are discussed and have largely been overcome using x-ray profile fitting software. The results show that when operated under optimum excitation conditions, ED-XRF spectrometry can routinely achieve a high degree of accuracy and precision in the analysis of a wide range of major and trace elements in silicate rocks. For many elements, 2s standard deviations are better than 2% relative. Limits of determination for many trace elements are in the range 4-10 ppm.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130103
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  • 205
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    Determination of the ash content of coal by multi-element x-ray fluorescence analysis (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 151-152 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A method for determining the ash content of coal by measuring the x-ray fluorescence of Si, Al, Ca and Fe using a diffraction spectrometer is presented. The experiments were carried out on 72 samples of coal from different deposits. A mean standard deviation of the ash content of about 1. 65% was achieved.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130404
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  • 206
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    PDIDENT - a set of programs for powder diffraction phase identification (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 172-179 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: PDIDENT is a collection of interactive computer programs which have been developed as aids for qualitative phase analysis of x-ray powder diffraction data. These FORTRAN IV programs are implemented on a DEC committee on Powder Diffraction Standards (JCPDS) data base is accessed by the programs along with user-created data. The data base (sets 1-32) along with all cross-index files requires 9 Mbytes of storage. The packing of the data base, use of cross-index files and the algorithms and utility of the PDIDENT programs are described.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130410
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  • 207
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    Compton scattering of x-rays: Some observations (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 192-194 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A set of experimental observations pertaining to Compton scattering of low-energy x-ray photons by matrices containing very light elements is reported.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130414
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  • 208
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    A fundamental parameter method for measurement of the thickness of pure element films by an EDX technique with a proportional detector (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 182-186 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Application of the fundamental parameter method to the determination of film thickness by an EDX technique with a proportional detector was performed by considering that x-rays striking the detector were composed of the following kinds: (1) the analyte line of the film excited directly by the primary beam, (2) the analyte line of the film excited secondarily by scattered or characteristic x-rays from the substrate and (3) scattered and characteristic x-rays from the substrate which passed through the film to be analysed. The intensity of all these types were considered theoretically, and the film thickness was evaluated by fitting the theoretical intensity of the x-rays striking the detector to the experimental intensity, by use of an iteration process. In addition, the accuracy of the theoretical values of intensities excited secondarily was verified by comparison with the experimental values.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130412
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  • 209
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    Melted sample (glass disk) ageing and its usability for x-ray emission spectrometry (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 148-150 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The usability of glass disks prepared from blast furnace slag samples as a function of age in x-ray emission spectrometry was investigated. Glass disks were prepared by melting sample and flux mixtures (Li2B4O7-Li2CO3-La2O3, 100: 10: 5) in the ratio 1: 100 at 1100°C for 30 min. The glass disks were examined by the ISIJ test. X-ray spectrometry and scanning electron microscopy were applied directly after preparation and again after 6, 12 and 18 months. A change in the surface of the glass disk and a decrease in the Ca Kα, Si Kα and S Kα line intensities with time were observed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130403
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  • 210
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    Quantitative light element analysis using an energy dispersive detector. 1-Dead time and the low-energy spectrum (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 69-77 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A study of the low-energy region (below 1. 5 keV) of energy dispersive x-ray spectra has been carried out. Firstly, because some counting systems do not provide a reliable dead time correction, a new method of dealing with the problem is given. Next, the effects of different positioning of the energy discriminator within the analyser circuitry are discussed with reference to the consequences for light element analysis. Electronic noise counts can present a problem for analysis of x-rays of less than 300 eV and a straightforward method for noise removal is described. Finally, an unexpected artifact in the spectrum below 500 eV is identified; its size is related to the total number of counts in the spectrum and a practical method of dealing with it is demonstrated. Once the above factors have been taken into account a low energy spectrum is produced, consisting solely of characteristic x-ray lines and a true continuum background.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130207
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  • 211
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    X-ray fluorescence analysis of iron ore concentrates (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 87-90 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: An x-ray method has been developed for the routine determination of many elements in iron ore concentrates. The combination of a glass disk technique, the α-coefficient method of correction and solution of linear equations yields a rapid and accurate method. The determination of eight elements was performed on different certified iron ore concentrates.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130210
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  • 212
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    Product news (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. viii 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130215
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  • 213
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    Masthead (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984) 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130301
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  • 214
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    Fundamental algorithm between concentration and intensity in XRF analysis 1 - theory (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 115-120 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A new formalism is proposed to correct with accuracy the matrix effects in x-ray fluorescence (XRF) analysis. It has been deduced from Sherman's equations and includes a new algorithm between concentration and intensity, theoretically exact, and explicit expressions permitting the calculation of αij and ρij coefficients that correct for absorption and enhancement effects, respectively. In other words, the concept of correction coefficients is established on a solid theoretical basis. In the second part, it will be shown how to adapt this new formalism to practical situations. From an estimate of composition calculated by the Claisse-Quintin algorithm and an appropriate calibration, the new algorithm is used to refine the estimated composition for greater accuracy. This last approach is equivalent to the ‘fundamental parameters’ method but is presented in a simpler version adaptable to any mini-computer.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130306
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  • 215
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    Spectral intensity distributions from x-ray tubes. Calculated versus experimental evaluations (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 134-141 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Apart from their general importance, an accurate definition of spectral intensity distributions from x-ray tubes is required to support the development of mathematical matrix correction procedures for x-ray fluorescence analysis. Since a direct measurement is costly, time consuming and occasionally difficult, and a purely theoretical approach is not suitable for current utilization, a simple, readily adaptable calculation procedure is very desirable. Concerning the continuum or white radiation from the x-ray tube, such an evaluation was worked out by effecting (1) a modification to Kramers' law and (2) a refinement of the absorption correction regarding the absorption by the target itself. The new equation accounts very closely for the best known, carefully measured and corrected experimental distributions by Brown et al. and Loomis and Keith. Extended experiments are required to ensure systematization, and special steps are needed for the treatment of the characteristic radiation.
    Additional Material: 15 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130309
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  • 216
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    Masthead (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984) 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130401
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  • 217
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    Study of some cobalt biomolecular complexes by x-ray absorption spectroscopy (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 153-155 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The fine structure in the vicinity of the K absorption edge of cobalt in some cobalt biomolecular complexes has been studied using a bent crystal x-ray spectrograph of the Cauchois type. The average metal - ligand bond length in these complexes has been determined by applying Levy's theory.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/xrs.1300130405
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  • 218
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    Computer method for qualitative wavelength-dispersive x-ray fluorescence analysis (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 187-191 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A computer method for the qualitative analysis of fluorescence spectra recorded with any analysing crystal and using any wavelength-dispersive x-ray spectrometer is described. Originally, the programs are designed for an Olivetti P 6066 computer without being on-line with the spectrometer. These programs may, of course, also be used with slight modifications with higher capacity and on-line computers, thus making the analysis easier and faster.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/xrs.1300130413
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  • 219
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    Product news (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. vi 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130114
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    Editorial (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 51-51 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130202
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    Trace element analysis of silicates by means of energy-dispersive x-ray spectrometry (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 64-68 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Three methods for the energy-dispersive x-ray spectrometric analysis of trace elements in silicate rock samples were compared. The comparisons were based on three new USGS reference samples, DNC-1, W-2, and BIR-1, and two established reference samples, G-1 and W-1. A loose powder sample preparation was used in the analysis of selected trace elements, including Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb and Ba. For one method, the ratio of analyte line intensity to either Compton or Compton and Rayleigh scatter intensity for a series of standards was used to construct calibration graphs. The other two methods involved fundamental parameter calculations which required a knowledge of the total sample compositions in order to perform the necessary matrix corrections. The results showed good accuracy for all three methods, but those obtained from the ratio-calibration graph method were slightly better than those from the other two methods.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/xrs.1300130206
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    Conference report (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. vi 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130212
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    Forthcoming meetings & conferences (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. vii 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130214
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  • 224
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    The stopping-power correction in proton-induced x-ray emission analysis (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 100-102 
    Details
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The thick-target yield of characteristic x-rays from a series of gold-silver binary alloys has been determined experimentally (relative to the yield from the pure elements) under proton bombardment, using proton energies of 1. 5, 2. 0 and 2. 5 MeV. The yield per unit concentration of gold or silver varies with alloy composition because of the progressively varying effects of proton stopping power (specific energy loss) and x-ray self-absorption in the target materials. Theoretical yields have been calculated using tabulated data for stopping power and x-ray absorption. When both of these effects are taken into account, agreement with experiment is satisfactory. These results can be made the basis of stopping power and self-absorption corrections in proton-induced x-ray emission analysis.
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    URL: http://dx.doi.org/10.1002/xrs.1300130303
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    Fundamental algorithm between concentration and intensity in XRF analysis 2 - practical applicationFor Part 1, see p. 115. (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 121-125 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: In Part 1, a new formalism was proposed to correct with accuracy the matrix effects in XRF analysis. In this paper it is shown how to adapt this new formalism to practical situations. From an estimate of composition calculated by the Claisse-Quintin algorithm and an appropriate calibration, the new algorithm is used to refine the estimated composition for greater accuracy. This last approach is equivalent to the ‘fundamental parameters’ method but is presented in a simpler version adaptable to any mini-computer.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/xrs.1300130307
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    Announcement (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. viii 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130312
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    Non-destructive measurement of gas pressures in sealed halogen lamps by x-ray spectrometry (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 170-171 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: X-ray spectrometry has been used to determine the pressure of krypton gas in high-pressure halogen auto lamps. The method employs a standard diffraction tube, a special collimator and a solid-state detector.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/xrs.1300130409
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    Theoretical evalution of the efficiency of compton scattered radiation method in EDXRF analysis (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 166-169 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A theoretical evaluation of the efficiency of correction for the matrix absorption effect using Compton scattered x-rays in EDXRF analysis has been carried out for thick samples and for monoenergetic primary radiation. The limitations of this correction method and the procedure for the selection of the optimum excitation energy are presented.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/xrs.1300130408
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    μ/ρ Algorithm valid for 1 keV ≤ E ≤ 50 keV and 11 ≤ Z ≤ 83 (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. 180-181 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Mass absorption coefficients can be calculated by this algorithm with programmable pocket calculators giving a standard deviation of about 5% when compared with McMaster's tables.
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    URL: http://dx.doi.org/10.1002/xrs.1300130411
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    Forthcoming meetings & conferences (1984)
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 13 (1984), S. viii 
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    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/xrs.1300130415
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    The analysis of trimethylamine in body fluids by a direct medium resolution mass spectrometric method (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 1-3 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple, high throughput method of analysis of trimethylamine in body fluids has been developed to assist with the management of patients with the inherited metabolic disorder, trimethylaminuria. The headspace in sealed vials was analysed using perdeuterated (2H10)trimethylamine hydrochloride as an internal standard. The gas chromatograph inlet system of the mass spectrometer was adapted to suit this method of analysis. Medium resolving power was used to measure the ion ratio of the [M-H]+ ion of trimethylamine and the [M-2H]+ ion of the internal standard. The method is faster and more accurate than gas chromatographic methods. The concentrations of trimethylamine found in normal urine are similar to those reported previously.
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    URL: http://dx.doi.org/10.1002/bms.1200110102
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    Analysis of peptides with unusual structural features by fast atom bombardment mass spectrometry: Protease inhibitors (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 10-23 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive ion and negative ion fast atom bombardment mass spectra of several natural and synthetic enzyme inhibitors are presented. It is shown that the fast atom bombardment method is well suited to the analysis of these unusual peptides. Complete amino acid sequences can be deduced from the mass spectra in most cases. Structural features typical of the inhibitors include (a) C-terminal aldehyde groups (e.g. leupeptin), (b) urea linkages in the peptide backbone (e.g. antipain, chymostatin), (c) prevalence of arginyl or α-(2-iminohexahydropyrimidyl)glycl residues, and (d) presence of an N-(glycosylphosphoryl) group (e.g. phosphoramidon). Several examples of synthetic peptides with common protecting groups are also presented. It is concluded that positive ion and negative ion fast atom bombardment mass spectra provide complementary information, the two techniques being sensitive to entirely different structural aspects of the inhibitors.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200110104
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    Microdetermination of 2-ketoglutaric acid in plasma and cerebrospinal fluid by capillary gas chromatography mass spectrometry; application to pediatrics (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 24-28 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Quantification of 2-ketoglutaric acid in plasma and cerebrospinal fluid as its O-trimethylsilyl-quinoxalinol derivative by gas chromatography chemical ionization mass spectrometry is described with benzoylformic acid as internal standard. This technique, with ammonia as reactant gas, only detects the protonated molecular ions. The recovery of 2-ketoglutarate from perchloric-deproteinized plasmas is 99.7±1.2%. The normal value of 2-ketoglutarate in children is 8.6±2.6 μmol I-1 (Mean ± standard deviation) in plasma (n =25) and 4.8±1.4 μmol I-1 in cerebrospinal fluid (n 20). The plasma level of 2-ketoglutarte is correlated with urea concentration (r = 0.96; p 〈 0.001) in healthy subjects and in patients with chronic renal insufficiency. Increased values are found in one case of pyruvate carboxylase deficiency, and inconstantly in diabetes; physiological variations are described during tasting and after an oral glucose load.
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    URL: http://dx.doi.org/10.1002/bms.1200110105
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    Field desorption mass spectrometry of anthracyclines comparison with other soft ionization techniques (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 35-40 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Field desorption mass spectral data relative to 38 anthracycline derivatives are presented. A molecular ion, or [MH]+ ion is always present; in most cases it is the base peak in the spectrum at the best anode temperature. Increase in the emitter temperature promotes fragmentation which gives useful structural information. A comparison has been made between field desorption and other soft ionization techniques such as fast atom bombardment, desorption chemical ionization and a liquid chromatographic mass spectrometric interface with direct liquid introduction into a chemical ionization ion source. The most significant results were obtained by using positive and negative ion fast atom bombardment and direct liquid introduction with negative ion detection.
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    Determination of betaxolol, a new beta-blocker, by gas chromatography mass spectrometry: Application to pharmacokinetic studiesA preliminary report was presented at the Fourth International Symposium on Quantitative Mass Spectrometry in Life Sciences - Gent, Belgium, 11-14 May, 1982. (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 29-34 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Betaxolol, a beta selective adrenoceptor antagonist recently approved for the treatment of hypertension, was determined by monitoring in chemical ionization mode with ammonia the [MH]+ ions of the trimethylsilyl derivatives of the drug and of its internal standard ((2H5)betaxolol). Its pharmacokinetic profile obtained following administration of a 20 mg oral dose was characterized by a half-life of 22 h and a bioavailability of 85%. The main acid metabolite formed by elimination of the isopropylamino group may also be determined as the methyl TMS derivative but methylation with BF3-methanol should be used with caution since it may induce the opening of the cyclopropyl group. The routine electron capture determination procedure was compared to this mass spectrometric method and an excellent correlation was found (r = 0.9974). Both procedures have the same sensitivity (1 ng ml-1). Finally it was observed that under electron impact mode betaxolol trimethylsilyl side chain rearranged to lose TMS—O—CH=CH2; this elimination was confirmed by deuterium labelling studies.
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    Fast atom bombardment mass spectrometry of nucleosides and nucleotides (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 41-46 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The positive and negative fast atom bombardment spectra of two nucleosides, 10 mononucleotides, two derivatized mononucleotides and 11 dinucleoside monophosphates have been recorded. Molecular ions (protonated or deprotonated) and some structurally significant fragments, sometimes involving cationization, were obtained. The spectra were compared with field desorption and thermospray ionization spectra whenever possible.
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    URL: http://dx.doi.org/10.1002/bms.1200110108
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    Masthead (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984) 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110201
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    Quantitative analysis of platelet activating factor (AGEPC) by fast atom bombardment mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 47-49 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Platelet activating factor has recently been structurally described as the phospholipid 1-O-alkyl-2-O-acetyl-sn-glycerophosphocholine. It has been reported to be a putative chemical mediator of immunological reactions as well as an antihypertensive agent. A method to quantitate 1-O-alkyl-2-O-acetyl-sn-glycerophosphocholine using deuterium labeled 1-O-alkyl-2-O-acetyl-sn-glycerophosphocholine as an internal standard is described. When 60 ng of the2H3 labeled compound is employed, quantities as low as 10 ng can be measured. The standard curve for this quantitative analysis typically had a correlation coefficient of 0.999 even when the signal saturation effect of FAB was apparent. Thus quantitative analysis using the FAB ionization technique is feasible when one employs the stable isotope internal standard method.
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    URL: http://dx.doi.org/10.1002/bms.1200110109
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    Determination of peptidoaminobenzophenone (2-o-chlorobenzoyl-4-chloro-N-methyl-N′-glycylglycinanilide) and its metabolites in human plasma by capillary gas chromatography negative ion chemical ionization mass spectrometry  -  2 (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 50-54 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capillary gas chromatographic negative ion chemical ionization mass spectrometric assay of peptidoaminobenzophenone (2-o-chlorobenzoyl-4-chloro-N-methyl-N′ -glycylglycinanilide) (1) and its three metabolites in human plasma reported in Part 1 was changed as follows: (1) the reagent gas was changed to ammonia from isobutane; (2) each unlabelled compound (1%) was added to the deuterium-labelled compound used as the internal standard; (3) all samples were injected in the splitless mode; (4) one more metabolite, lormetazepam, was determined; (5) day-to-day reproducibility was checked in the range of 1-50 ng ml-1. Points 1 to 3 improved the preciseness with small-sized samples. Calibration curves were prepared in the range of 0.5-50 ng ml-1. Plasma levels of compound 1 and its four metabolites in 10 volunteers were measured.
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    Fast atom bombardment mass spectrometry of insulin, insulin A-chain, insulin B-chain, and glucagon (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 55-59 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment mass spectral data are presented for the polypeptides insulin, oxidized insulin A-chain, carboxymethylated insulin B-chain, and glucagon. The doubly-charged molecular ion of the intact insulin molecule produced with fast atom bombardment with xenon atoms is observed at a reduced accelerating voltage (4 kV).
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    URL: http://dx.doi.org/10.1002/bms.1200110202
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    The identification of C-18 neutral steroids in normal stallion urine (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 96-99 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: As part of a continuing research program associated with the detection of anabolic steroid residues in horse urine,1-8 normal samples from entire male horses have now been investigated. Isomers of three C-18 neutral steroids; 4-estron-17-ol-3-one (1), estrane-3,17-diol (2) and an unsaturated estranediol having a possible structure (3), have been identified in urine samples from two male horses aged 8 and 14 years. Of these three steroids, compound (2) was not detected in the urine of a 2.5 yr old entire male nor in the majority of post-race urine samples from entire male horses average age 3.8 yrs (n = 34). Ten of these samples showed tentative indications of this compound. Although the isolation of isomers of estrane-3,17-diol from human non-pregnancy urine has been reported previously,9 analysis of non-pregnancy urine samples in the present study did not reveal the presence of these compounds.
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    URL: http://dx.doi.org/10.1002/bms.1200110209
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    Mass spectrometry of the copper salt of tenuazonic acid (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 101-105 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The copper salt of tenuazonic acid was studied by both positive and negative ion techniques. Fragmentation was elucidated with the aid of collision-induced dissociation/mass-analysed ion kinetic energy spectroscopy. During the course of the investigations, a homolog of tenuazonic acid was tentatively identified by using a combination of mass spectral techniques.
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    URL: http://dx.doi.org/10.1002/bms.1200110302
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    Analysis of moth pheromone acetates by selected ion monitoring using electron impact and chemical ionization mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 106-113 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass spectrometric determination of moth pheromone components by means of selected ion monitoring with electron impact and chemical ionization has been evaluated. For the analysis of acetates, chemical ionization with ammonia as reactant gas proved advantageous with respect to sensitivity and selectivity. A quantitative assay for determination of pheromone samples from individual turnip moth females (Agrotis segetum, Noctuidae), using internal standards, deuterated at the acyl group, was developed. The assay showed correct linearity in the investigated region (20-2000 pg). Signal to noise ratios for 100 pg of acetates using chemical ionization (ammonia as reactant gas) were in the range 10-50 depending on the degree of unsaturation. Conservative limits of detection (background signal + three times the standard deviation) and quantification (background signal + 10 times the standard deviation) were approximately 70 and 240 pg, respectively. A significant decrease in gland titre of (Z)-5-decenyl acetate and (Z)-7-dodecenyl acetate after mating was established.
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    URL: http://dx.doi.org/10.1002/bms.1200110303
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    A PGE2-derivative for quantitative gas chromatographic mass spectrometric measurement in the selected ion monitoring modePresented in part at the 21st Annual Meeting of the German Pharmacological Society, Mainz, March 1980 (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 114-117 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The quantification of prostaglandin PGE2 by gas chromatography mass spectrometry in the form of an easily prepared derivative is described. After extraction and purification of biological samples the compound was derivatized in two steps to 9-enol-PGE2-methylester-trimethylsilylether, 9-enol-PGE2 -Me-TMS3. The molecular ion at m/z 582 with 40% relative abundance and the fragment ion at m/z 492 with 100% relative abundance permit a specific and sensitive evaluation in the selected ion monitoring mode. The high masses selected lie above the biological background. The calibration curve produced by adding known amounts (10-200 ng) of PGE2 to blank human urine and with (2H4)-deuterated PGE2 as internal standard gave a linear correlation. The separation from biological impurities was obtained on a 50 m glass capillary column and resulted in sharp and symmetrical peaks.
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    Putrescine metabolism: Enzymatic formation and non-enzymatic isotope exchange of Δ′-pyrroline (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 118-120 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The deamination of putrescine catalysed by diamine oxidase was carried out in deuterium oxide and deuterated buffers. Enamine and α,β-unsaturated intermediates were excluded, based on the observation that deuterium was not incorporated into Δ1-pyrroline during its enzymatic formation in deuterium oxide. When the reaction mixture was buffered with phosphate, isolated Δ1-pyrroline contained two deuterium atoms at C-3, indicating that a phosphate-promoted, non-enzymatic isotope exchange had occurred. Using 5,5-dimethyl-Δ1-pyrroline as a model compound, the nature of the non-enzymatic deuterium exchange was studied and a bifunctional catalysis mechanism proposed. The results suggest that the choice of buffer could alter the conclusions drawn from enzyme mechanism studies involving imine-enamine tautomerism.
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    URL: http://dx.doi.org/10.1002/bms.1200110305
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    Determination of metabolites of 3-chloro-4-benzyloxyphenylacetic acid (benzofenac) by GC/MS method (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 121-126 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metabolites of benzofenac (3-chloro-4-benzyloxyphenylacetic acid) were determined in rat, rabbit, dog, and human urine by GC/MS. Before analysis the urine was extracted and the extracts were treated with diazomethane. Deuterium-labelled benzofenac, 3-chloro-4-([methylene-2H2]-benzolyoxy) phenylacetic acid was used for the elucidation of the structures of some main metabolites and the determination of trace metabolites. The structures of the metabolites were determined from spectra obtained by electron impact and chemical ionization.
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    URL: http://dx.doi.org/10.1002/bms.1200110306
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    Laser desorption mass spectrometry of synthetic lipid a-like compounds (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 132-141 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The applicability and the present limitations of the laser microprobe mass analyser LAMMA®-500 as an instrument for the structural analysis of higher molecular weight, non-volatile, bio-organic compounds (≤2000 u) were investigated. For this purpose mass spectra of various synthetic and natural compounds representing cell wall components of Gram-negative bacteria, e.g. phospholipids and lipid A-like molecules were studied. In several cases these spectra exhibited relatively simple and interpretable patterns with a prominent quasi-molecular ion originating from alkali attachment. For one group of the compounds studied - synthetic lipid A-like molecules containing a phosphate moiety - the spectra were rather complicated and lacked pronounced quasi-molecular peaks. Possible reasons for this observation are discussed.
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    Characterization of double bond positions in dodecenols by electron impact mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 145-148 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The positional isomerism of seven dodecenols (Δ5-Δ11), without any prior chemical modification, was clearly elucidated by the conventional combined gas chromatography electron impact mass spectrometry. The relative abundances of some predominant fragment ions in the isomers examined were governed by the position of the original double bond. The intensity ratios of certain selected pairs of predominant ions are of diagnostic value for the determination of the double bond position. A procedure for the location of the double bond position is given.
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    Masthead (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984) 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110401
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    Measurement of endogenous tryptamine in rat brain by capillary column gas chromatography mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 155-158 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary column gas chromatographic mass spectrometric method, involving the use of a deuterated analogue as internal standard, was developed and used to identify and quantify tryptamine in the rat brain. The mean level of tryptamine i rat whole brain was 0.54 pmolg-1.
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    Biliary excretion of hydroxyethyl starch in man (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 164-166 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The extent of biliary excretion of hydroxyethyl starch (HES) in man after intravenous administration of 500 ml of a 6% solution to nine healthy male volunteers was determined using a specific gas chromatograph mass spectrometer selected ion monitoring procedure. On the average, less than 1% of the administered dose was recovered in feces over a 14 day period.
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    URL: http://dx.doi.org/10.1002/bms.1200110405
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    Mass spectrometry of 2-substituted-4-arylthiazoles. 3 - identification of microsomal nitroreduction products by mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 149-154 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact mass spectra of the chemical carcinogens 4-(4-aminophenyl)-2-methylaminothiazole, 4-(4-aminophenyl)-2-methylaminothiazole, and 4-(4-aminophenyl)-2-aminothiazole were studied. The 3-(4-aminophenyl)-2-substituted thiazoles were isolated from the anaerobic microsomal reduction of their respective 4-nitrophenyl analogues. Microsomes prepared from rat and rabbit kidney tissues were used. The identity of the reduction products were established by chemical synthesis and mass spectrometry. The mass spectrometric fragmentation of the nitro derivative shows prominent ions arising from the loss of the nitro group, ring enlargement of the thiazoles, and the phenylthiirene ion resulting from 1,2-cleavage of the thiazole ring. In the 4-(4-aminophenyl)-2-substituted amino derivative prominent ions result from the preferential 1,2-cleavage of the thiazole ring to give the common 2-(4-aminophenyl) thiirene ion and subsequent fragmentation of this ion.
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    Laser microprobe mass spectrometry of platinum in dog kidney after cisplatin adminstration (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 159-163 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By means of laser microprobe mass analysis (LAMMA) platinum was detected in the renal proximal tubular cells of a dog that had been intravenously adminstered the antitumor drug cisplatin (5 mg per kg body weight). No definite subcellular localization of the heavy metal was obtained. Sample prparation and analytical features are examined to increase spatial resolution of analysis while maintaining sufficient detection efficiency. The LAMMA method is destructive, but the amount and type of evaporated material can readily be determined when using LAMMA in combination with transmission electron microscopy. Instrumental optimization and standardization of mass signals is possible by using platinum-loaded, ion chelating resin beads embedded and sectioned with the tissue.
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    Chemical ionization mass spectrometry of iprodione and its metabolites (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 589-593 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: One of the cornerstones of an architectural approach adopted by this laboratory in screening vegetables for pesticides and industrial chemicals is the extensive use of element-selective gas chromatographic detectors followed by gas chromatography/mass spectrometry. In this particular case history, a recently introduced European fungicide, iprodione, was thought to be the first reported incidence in mache imported from France. An analytical protocol involving chemical ionization was devised to confirm this finding as well as search for possible potential metabolites.
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    Metabolic studies of explosives. 1 - EI and CI mass spectrometry of metabolites of 2,4,6-trinitrotoluene (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 594-600 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of metabolites of trinitrotoluene (TNT) have been synthesized and analysed by electron impact (EI) and chemical ionization (CI) mass spectrometry. Identification characteristics of these metabolites by their mass spectra have been determined. Differentiation of isomers is made possible by EI ions which are characteristic of the position of the methyl group with regard to the nitro groups.
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    Letter to the editors (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 601-601 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200111109
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    Gas chromatographic/mass spectrometric method for the identification of Δ5,7-sterols in sterol mixtures (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 608-610 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple method for gas chromatographic/mass spectrometric identification of Δ5,7-sterols and their acetates in complex sterol mixtures is proposed. It is based on the fact that they are more readily dehydrated (respectively deacetylated) at high temperatures, compared with Δ5-sterols. Sterol mixtures from four marine invertebrates were investigated by this method.
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    Mass spectral and HPLC analysis of biological compounds with diphenylborinic acid (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 611-615 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diphenylborinic acid is shown to react with a variety of polyfunctional molecules of biological interest to give products which are easily identifiable by mass spectrometry. The diphenylborinate adducts of amino acids possess extraordinary stability and are separable by reverse phase chromatography. The stability of products is discussed with regard to the nature and stereochemical arrangement of the functional groups involved in complex formation.
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    A comparison of thermospray and direct liquid introduction high-performance liquid chromatography/mass spectrometry for the analysis of candidate antimalarials (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 616-621 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of antimalarials by high-performance liquid chromatography (HPLC)/mass spectrometry demonstrates a new dimension in specificity along with increased sensitivity compared to conventional HPLC detection methods. Both direct liquid introduction and thermospray HPLC/mass spectrometry interfaces provided molecular weight information as well as characteristic fragment ions for antimalarials not normally amenable to direct probe or gas chromatographic/mass spectrometric techniques. The direct liquid introduction interface, which incorporated a 1/100 split, showed a detection limit of 30 ng using selected ion monitoring. The thermospray technique showed less than 1 ng detection limits using selected ion monitoring.
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    Fast atom bombardment mass spectrometry and tandem mass spectrometry in antibiotics: Identification of nucleoside antitumor antibiotic toyocamycin in fermentation brothSee Ref. 1. (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 622-628 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The presence of the nucleoside antitumor antibiotic toyocamycin in the fermentation broth was determined by a combination of negative and positive ion fast atom bombardment (FAB) mass spectrometry, high resolution FAB mass spectrometry and mass-analysed ion kinetic energy spectrometry (MIKES). A reasonable limit of detection for toyocamycin in the whole broth was obtained by combining the specificity of mass spectrometry/mass spectrometry (also called tandem mass spectrometry) to FAB. The role played by the fermentation matrix upon the production and the observation of characteristic ions by FAB. using xenon atoms was examined. High-performance liquid chromatography (HPLC) and FAB mass spectrometry were used to monitor toyocamycin at all stages of strain development, fermentation and recovery.
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    Determination of plasma bupropion and its relationship to therapeutic effect (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 629-632 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analytical method to determine the concentration of bupropion in human plasma has been developed using a deuterium-labeled analog as internal standard and selected ion monitoring applied to an extract of plasma samples taken as part of a clinical trial of this antidepressant. In all, 15 depressed outpatients were randomly assigned to bupropion in a double-blind study which included weekly evaluation of their clinical condition. A good correlation was found between the results obtained by this assay and by a radioimmunoassay technique currently in use. While no simple correlation between plasma concentration and therapeutic improvement was noted, the majority of subjects showed mild to marked amelioration of symptoms and those having mean concentrations above 35 ng ml-1 had significant improvement in their test scores. Interpretation of the mass spectra of both the labeled and unlabeled drug revealed an apparent violation of the ‘even-electron rule’.
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    Electrospray mass spectroscopy of macromolecules: Application of an ion-drift spectrometerThis paper was invited by the Editor at the time of Professcr Dole's retirement. (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 259-268 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Macroions of lysozyme and polystyrene produced by the electrospraying of dilute solutions of these macromolecules into nitrogen gas at atmospheric pressure have been studied by means of the measurement of their mobilities in nitrogen by means of an ion-drift spectrometer. In the case of polystyrene mainly clusters of negative macroions have been detected and studied, but in the case of lysozyme macroions containing one, two or three positive charges can be identified. The effect of change of solution concentration, temperature and pressure in the ion-drift tube on the data obtained in the case of polystyrene has been observed.
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    Silver sulfonates as mass standards in field desorption mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 273-275 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two commercially available compounds, silver methanesulfonate and silver trifluoromethanesulfonate, and a mixture of these compounds are useful as mass standards in field desorption mass spectrometry, offering certain advantages over compounds and methods currently being used for this purpose. These mass standards can be utilized in calibrating or confirming the accuracy of a data system or a mass marker calibration and for peak matching up to a mass of about 1440.
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    Quantitative determination of nitroglycerol in human plasma by gas chromatography negative ion mass spectrometry using 15N labelled nitroglycerol as internal standard (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 276-277 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Negative ionization resulted in the simplification of a previously published method. The new method permits the determination of 0.25 nmol l-1 nitroglycerol in plasma with a coefficient of variation of 9.1%.
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    Chenodeoxycholic acid pool size determination from children using isotope dilution mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 269-272 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An isotope dilution mass spectrometry method is described for determining chenodeoxycholic acid pool size in children. The stable isotopically labeled tracer. (11,12-2H2) chenodeoxycholic acid, was administered orally to children, and the enrichment of bile was measured by selected ion monitoring gas chromatography mass spectrometry. The level of (11,12-2H2) chenodeoxycholic acid enrichment found in the patient samples was in the range of 0.5 to 5%. Data are presented illustrating the duplication of this method in two independent laboratories using standard quadrupole mass spectrometers. This procedure provides the clinician with a non-radioactive method for determining chenodeoxycholic acid pool size which is especially beneficial in studies involving children and pregnant women.
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    Chemical ionization mass spectrometry of carbamates. 1 - N-phenylcarbamates - propham and chlorpropham (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 301-307 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Under ammonia and methane chemical ionization conditions, using a liquid chromatographic moving belt interface for sample introduction, molecular weight information has been observed for two representative N-phenylcarbamates, propham (isopropyl N-phenylcarbamate) and chlorpropham [isopropyl N-(3-chlorophenyl)carbamate]. Displacement reactions can occur in which the side-chain is expelled as a neutral olefin via a hydrogen rearrangement. The temperature dependence of these spectra has been studied and the relative concentration of [MH]+ ions increases with decreasing temperature.
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    Masthead (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984) 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110701
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    On-line liquid chromatographic/mass spectrometric studies using a moving belt interface and negative chemical ionization (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 308-309 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Using the new Finnigan moving belt liquid chromatographic/mass spectrometric interface some cardiac glycosides and oligosaccharides have been reinvestigated using C1- negative chemical ionization. Abundant [M+CI]- ions are found with all cardiac glycosides and raffinose.
    Additional Material: 2 Ill.
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    Fast atom bombardment mass spectrometry of the muscarosides. An aid to the glycoside sequence determination (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 310-314 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structure elucidation of a novel branched-chain hexasaccharide glycoside, muscaroside B, has been aided by fast atom bombardment mass spectrometry Muscaroside A - a straight-chain analogue having the same 27-norlanostane skeleton and spirofused tetrahydrofuran ring - and digitonin - a branched-chain steroidal glycoside -  were used as standards.
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    A new look at the mechanism of chemical ionization fragmentation of demethylated choline esters (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 315-319 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mechanism of fragmentation in the chemical ionization mass spectra of thermally demethylated choline esters has been investigated using various deuterated analogs of acetylcholine as models. The reagent gases employed included CH4, C2H4, NH3 and N2H3. Prominent [MH]+ or [M2H]+ ions were observed respectively in all cases. A 1,3-hydrogen rearrangement in the acetyl portion followed by loss of ketene was seen in CH4 chemical ionization spectra, as well as cleavage of the CH2—N bond after protonation on the nitrogen. Alpha cleavage produced ions analogous to the m / z 58 ion which is found as the base peak in the electron impact spectra of demethylated choline esters. A major difference between the fragmentation after electron impact and chemical ionization was seen in the m/z 72 region. The McLafferty rearrangement observed after electron impact was not found after chemical ionization. Rather, a mechanism involving protonation of the carboxyl group followed by simple cleavage of the CH2—O bond was consistent with the present results for the variously labelled analogs and reagent gases. Finally, in the chemical ionization mass spectra of demethylated acetylcholine little retention of the H+ or 2H+ was found in the observed fragment ions.
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    Capillary gas chromatographic/mass spectrometric analysis of abnormal metabolites in hypoglycin-treated rat urine (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 332-339 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Numerous abnormal metabolites were identified in large amounts in the urine of hypoglycin-treated rats using capillary gas chromatography/mass spectrometry-computer analysis. These metabolites are not detectable in significant amounts in normal rats' urine. Ten of them have not been previously associated with hypoglycin administration: these are several hydroxy compounds, including those from the valine and isoleucine pathways, 2-oxo-adipic acid, n-butyrylglycine and isovaleryl glucuronide. These results indicate that the pathways of isoleucine and valine netabolism are inhibited at their respective acyl-CoA dehydrogenation steps, as is the case for fatty acid, leucine and lysine metabolism, as previously shown. The mass spectra of the trimethylsilyl derivatives of cis, cis-4,7-decadiene-1,10-dioic, cis-4-decene-1,10-dioic, cis-4-octene-1,8-dioic acids, and (methylenecyclopropyl)acetylglycine, which were previously identified using nuclear magnetic resonance and oxidative cleavage or acid hydrolysis, are presented for the first time.
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    Evidence for the in vitro metabolism of allylisopropylacetamide to reactive intermediates. Mechanistic studies with oxygen-18 (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 320-331 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metabolism of allylisopropylacetamide (AIA) (1) in microsomal preparations from phenobarbital-pretreated rats is shown to proceed by way of three cytochrome P-450-dependent pathways: (i) aliphatic (C-3) hydroxylation, (ii) allylic (C-3) hydroxylation and (iii) olefin oxidation. The latter represents the major route of biotransformation and leads ultimately to the formation of the γ-butyrolactone 2. In order to elucidate the mechanism by which AIA is converted to this γ-Iactone, and to gain information on the nature of chemically reactive intermediates in the process, the metabolism of AIA to 2 was investigated in 18O2 or H218 O and the pattern of label incorporated into the product was determined by gas chromatography/mass spectrometry (GC/MS). The results support the formation of AIA epoxide as an initial product of olefin oxidation and indicate that this species undergoes rapid intramolecular rearrangement to a protonated iminolactone which, in turn, is hydrolysed to the stable γ-lactone. On the other hand, the ‘dihydrodiol’ metabolite of AIA, which would be expected to result from direct hydrolysis of AIA epoxide, was not detected in incubation products and, furthermore, the 18O labeling data specifically exclude the possibility that it served as a precursor of 2. It may be concluded, therefore, that AIA epoxide and the protonated iminolactone to which it gives rise represent reactive intermediates in the oxidation of AIA which may play a key role in the alkylation of certain cellular constituents which accompanies metabolism of AIA by liver enzymes.
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    Picolinyl derivatives for the structural determination of fatty acids by mass spectrometry: Applications to polyenoic acids, hydroxy acids, di-acids and related compounds (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 340-347 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A rapid, mild procedure is described for the synthesis of picolinyl esters of branched-chain, cyclic and unsaturated fatty acids, dicarboxylic acids and hydroxy acids by the reaction of the derived acid chloride with 3-pyridylcarbinol. The mass spectra of these derivatives contained abundant diagnostic ions resulting from radical-induced cleavage of the hydrocarbon chain following random hydrogen abstraction by the nitrogen atom of the pyridine ring. Ions thus represented cleavage, without further rearrangement, at each carbon-carbon bond and enabled methyl groups and double bonds to be located. The spectra of the polyenoic acids were more complex than those of their monoenoic analogues, but major ions whose mass differences could be represented by the series  - 14, 26, 14, 26, 14 -  could be used to localize the double bonds. The position of the double bond most remote from the carboxylic ester group could be established by the position of an abundant ion produced by loss of an allylic radical containing the terminal carbon atoms of the chain. Derivatives of the hydroxy acids, although not prepared in quantitative yield, also gave diagnostic spectra. The spectra of the derivatives of the dicarboxylic acids contained abundant molecular ions and again showed diagnostic cleavages of the hydrocarbon chain.
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    Preparation of CO2 from blood and protein-bound amino acid carboxyl groups for quantification and 13C-isotope measurements (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 348-352 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Measurements of protein and amino acid metabolism in man using stable isotopes and selected ion monitoring gas chromatographic/mass spectrometric techniques are limited by the requirement of relatively high levels of labelling for adequate precision ( 〉 0.05 at % excess). We describe here a means of extending the scope of such studies by measurement of lower levels of enrichment achieved in gaseous CO2 derived from whole blood or protein-bound amino acids following the administration of tracer amounts of appropriately labelled substrates. Construction and operation of a novel glass vacuum line required for this work are described in detail and specific applications relevant to clinical investigations are outlined. Measurements of both the total amount of CO2 and its 13C enrichment are performed in an isotope-ratio mass spectrometer which provides acceptable levels of accuracy and reproducibility for both measurements ( ±0.1% and ±0.0001 at% excess respectively).
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    Comparison of derivatives for the characterization of branched long-chain alcohols and 1,2-diols by mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 353-359 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trimethylsilyl (TMS) ethers, acetates, cyclic alkane boronates (of diols) and nicotinates were evaluated as derivatives for determining the structure of n-, iso- and anteiso- long-chain alcohols and 1,2-diols. The nicotinates were the most satisfactory for both the mono- and dihydric compounds; their spectra contained a series of ions produced by radical-induced cleavage following random hydrogen abstraction from the aliphatic chain, and the differences in relative abundances of these ions reflected the position of methyl branching. In the spectra of all the derivatives studied, ions at m/z 56 and 70 were characteristic of the iso- and anteiso-structures respectively, but only in the spectra of the acetates of the monohydric alcohols were the relative abundances of these ions diagnostically useful. The cyclic alkane boronates were found to be poor indicators of chain structure. Several new fragmentations of the TMS derivatives of primary alcohols are reported.
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    The identification of cyclic nucleotides from living systems using collision-induced dissociation of ions generated by fast atom bombardment mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 367-374 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Extracts derived from rat liver and Phaseolus leaves are shown, by collision-induced dissociation of [MH]+ ions generated by fast atom bombardment mass spectrometry, to contain cytidine 3′,5′-cyclic monophosphate and guanosine 3′,5′-cyclic monophosphate respectively, and not the 2′,3′-cyclic isomers. Interference peaks, expected to be common to all mass-analysed ion kinetic energy spectra of ions generated by the fast atom bombardment process from glycerol-based matrices are identified. It is shown that unequivocal identification of cytidine 3′,5′-cyclic monophosphate can be made at the microgram level. Attempts to derive a quantitative procedure based on using different cyclic nucleotides as internal standards were unsuccessful due to the poor solubility of these compounds in the matrix system.
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    A mass spectral study of cyclophosphamide with special reference to differences in isomeric structures (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 360-366 
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    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass spectrometric fragmentation of cyclophosphamide (CP) has been studied in detail using linked field scanning, isotope labelling, low energy ionization and accurate mass measurements. The molecular ion is of low abundance and it favours loss of HCI and ·CH2CI to form the base peak at m/z 211. All the other ions are formed by sequential fragmentation processes. The direct bond rupture between phosphorus and the N-chloroethyl group produces two ions m/z 120 and m/z 92. The ion m/z 56 is a triplet. Many of the ions in the spectrum are produced by several competing pathways. Several of the rearrangement mechanisms involve a single hydrogen transfer. Quantitative differences between two commercial CP preparations were observed in the linked field scanning spectra. Differences in the abundances of the metastable ions strongly suggest that there is an intense isomeric competition in the decomposition pathways. The experimental evidence supports the conclusion that the two CP preparations differ in their isomeric composition and these differences are related to their stereoisomers. The rates of the individual fragmentation pathways are dependent upon the isomeric structure of the parent molecule and might also be reflected by different rates of metabolism of the isomers of the drug in vivo.
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    Fast atom bombardment mass spectrometry of cyanogenic glycosides (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 375-376 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The potential of positive and negative Ion fast atom bombardment mass spectrometry in the examination of cyanogenic glycosides has been demonstrated by the analysis of linamarin, prunasin, neolinustatin and amygdalin.
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    Forthcoming meetings (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. i 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110711
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    Masthead (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984) 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110801
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    Structure determination of phospholipids by secondary ion mass spectrometric techniques: Differentiation of isomeric esters (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 383-385 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The secondary ion mass spectrometry, regardless of the charge status of the primary beam, is a good means not only of determining the type of phospholipid and the fatty acid components but also the isomeric positions of the acyl groups. Matrix-assisted secondary ion (SI) mass spectra of phosphatidylcholines in the positive mode show two characteristic doublets 2 u apart originating from the deacyl and deacyloxy cleavages of the compounds. The relative abundance of these ions is diagnostic of the ester positions, that is, the fragments originating from the C2-ester loss are more abundant than the corresponding ones from the C1-ester loss.
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    Secondary ion mass spectra of tryptic peptides of human hemoglobin chains (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 386-391 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Secondary ion mass spectra of tryptic peprides of human globin α-, β-, γ and α-chains were studied. Almost all mass peaks of protonated molecular ions of tryptic peptides were observed and they were very stable and abundant. The present results show the possibilities for quantitative analysis of two γ-globin species: Aγ and Gγ chains, and for structural analysis of unknown abnormal hemoglobins.
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    Diethylsilyl ether and diethylsiliconide derivatives in gas chromatography mass spectrometry of hydroxylated steroidsA part of this paper was presented at the 29th Annual Conference on Mass Spectrometry and Allied Topics, Minneapolis (1981). (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 377-382 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The gas chromatographic and mass spectrometric properties of the diethylsilyl (DEHS) or diethylsiliconide (DES)-DEHS ether derivatives of 20 hydroxysteroids of various types have been studied using N,O-bis(diethylsilyl)trifluoroacetamide as a new silylating agent. The mass spectra of the DES-DEHS ether derivatives were characterized by their marked simplicity and by molecular ions of high abundance, whereas the mass fragmentation patterns of the DEHS ether derivatives without formation of the DES group in the molecule were similar to those of the corresponding dimethylethylsilyl (DMES) ether derivatives. The appearance of the molecular ion may be very useful for estimating the molecular weight of hydroxysteroids of which other silyl ether derivatives yield molecular ions of insufficient abundance to characterize them. In particular, the DES-DEHS ether derivative of 5β-pregnane-3α,17α,20α-triol gave the molecular ion at m/z 506 as a principal ion in the electron impact ionization mode. The methylene unit values of the DEHS ether derivatives of hydroxysteroids without formation of DES groups were slightly larger than those of the corresponding DMES ether derivatives. A Δ[Um]s value was presented for estimation of the number of siliconide moieties in the DES-DEHS ether derivatives.
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    Enzyme reaction rates determined by fast atom bombardment mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 392-395 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) mass spectrometry has been used to measure the reaction rate of trypsin with the synthetic substrate p-toluenesulfonyl-L-arginine methyl ester (TAME). Rates were measured by FAB mass spectrometry both in real time by monitoring the reaction as it proceeded on the probe inside the mass spectrometer, and also by individual analysis of a series of aliquots removed with time from a batch reaction. The results were then compared to the rates measured using the usual spectrophotometric (UV) assay run with the same reaction mixture. The results showed that the initial rates of trypsin cleavage were the same for these three methods at approximately 0.15 μmol product produced min-1 μg-1 enzyme. After 5 min, the rates determined by FAB mass spectrometry using timed aliquots and the UV assay remained about the same, whereas the real-time measurement decreased substantially to approximately 0.002 μmol product min-1 μg-1 enzyme. The results are discussed with respect to the particular advantages and disadvantages of these methods for following enzyme reactions.
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    PAAS 3: A computer program to determine probable sequence of peptides from mass spectrometric data (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 396-399 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The computer program PAAS 3 is developed to determine the probable amino acid sequences of a peptide from sequence ion peaks experimentally obtained by mass spectrometry.
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    URL: http://dx.doi.org/10.1002/bms.1200110806
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    Fast atom bombardment mass spectrometry of metal nucleotide complexes (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 400-402 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Fast atom bombardment mass spectrometry of the beta-gamma complexes of ATP and GTP with cobalt and chromium are reported. Spectra were recorded in the positive ion mode. Ions in the molecular weight region allow identification of the complexes to be made.
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    URL: http://dx.doi.org/10.1002/bms.1200110807
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    Direct monitoring of sequential enzymatic hydrolysis of peptides by thermospray mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 403-407 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A procedure for peptide sequencing using an immobilized exopeptidase column directly coupled to a thermospray mass spectrometer is described. The amino acids sequentially released from the C-terminus of the peptide chain are directly introduced into a thermospray ion source by a flowing aqueous buffer. The buffer is essential for the direct production of ions from solution. The method eliminates the need to derivatize the amino acids for detection and, by comparison to standard injections, amino acid sequence information can be obtained in less than two minutes. With the present configuration, detection limits are typically in the low picomolar range.
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    Electron impact mass spectrometry of some amino derivatives of 1,4-benzodiazepines (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 408-414 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact mass spectra of some mono- and diamino derivatives of 5-phenyl-1,4-benzodiazepines have been determined, and their fragmentation pattern elucidated with the aid of deuterium-labelled derivatives, high resolution mass measurements and metastable analysis. The most significant ions are derived from the loss of the amino residues, and from the contraction of the seven-membered benzodiazepine system to give smaller rings.
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    URL: http://dx.doi.org/10.1002/bms.1200110809
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    Approaches to the improvement of quantitative precision in selected ion monitoring: High resolution applications (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 415-420 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A MAT 731 mass spectrometer has been modified to permit multiple ion monitoring at resolutions of 8000-10 000. The greater imprecision in response ratio (analyte/internal standard) determinations which accompanies the increase in mass spectrometric resolution is attributable to the weaker signal detected, rather than to instrument instability. The mass spectrometer has been coupled to a microprocessor-based data system and software prepared to facilitate the precise determination of response ratios. Imprecision is markedly reduced when isotope ratios are determined by linear regression analyses of signals attributable to the two ionic species detected.
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    Development of a gas chromatographic selected ion monitoring assay for thyroxine (T4) in human serum (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 421-427 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The components of a gas chromatographic mass spectrometric-selected ion monitoring (SIM) assay for thyroxine (T4) in human serum are described. The internal standard for the assay was synthesized from deuterium-labelled 3,5-diiodotyrosine and 3,5-diiodo-4-hydroxyphenylpyruvic acid. A novel method was developed for isolating the products of the coupling reaction. The results obtained by gas chromatography mass spectrometry SIM were compared with those of radioimmunoassay. The gas chromatographic mass spectrometric SIM assay would form the basis of a reference assay for T4.
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    Masthead (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984) 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110901
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    Diastereoisomeric determination of R-alanine in bacteria using capillary gas chromatography and positive/negative ion mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 428-434 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The possibilities of using combined capillary gas chromatography mass spectrometry for highly sensitive and selective determinations of enantiomeric alanines of bacterial origin have been evaluated. The alanines were separated as their diastereoisomeric N-heptafluorobutyryl-2-butyl ester derivatives on a 25 m fused silica capillary column coated with SE-54 as stationary phase. The mass spectra of the derivative obtained by chemical ionization using methane or ammonia (positive ions) and methane or Isobutane (negative ions) as reagent gases have been recorded. The highest sensitivity of detection was achieved by selected ion monitoring in the negative ion mode (detection limit about 0.8 pg). The method was tested by measuring the R-alanine content in (a) Escherichia coli cultures and (b) natural bacterial communities associated with plant roots. In (a) the recorded detection limit implied possibilities to detect R-alanine corresponding to 103-104 E. coli cells. The precision for quantifying R-alanine in the cultures was 14% (coefficient of variation). (b) demonstrated an application where the R/(R + S) ratio of alanine is low. It was shown that accurate determinations of this ratio in the picogram range could be effected down to 0.4%.
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    Bis(trifluoromethyl)aryl derivatives for drug analysis by gas chromatography electron capture negative ion chemical ionization mass spectrometry. Application to the measurement of low levels of clondine in plasma (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 435-440 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic mass spectrometric assay for clonidine in plasma with a detection limit of a few picograms per ml was required. The p-trifluoromethylbenzyl, pentafluorobenzyl and pentafluorobenzoyl derivatives of clonidine were synthesized and the electron capture negative ion chemical ionization mass spectra of these compounds show extensive fragmentation with prominent ions at m/z 35 and 37 due to the two chlorine atoms in the clonidine molecule. Selected ion monitoring of specific high mass ions in these mass spectra indicated that the required sensitivity could not be obtained with these derivatives. Several bis(trifluoromethyl)pyrimidines were synthesized and these compounds were found to give an intense negative ion current under conditions of resonance electron capture. Consequently, a derivative of clonidine containing a bis(trifluoromethyl)aryl group was synthesized by reacting the drug with 3,5-bis(trifluoromethyl)benzoyl chloride. The negative ion mass spectrum of the reaction product has a base peak at m/z 673 and, when this ion is specifically monitored, an amount of derivative equivalent to 1 picogram of clonidine can be detected. This allowed the development of an assay for clonidine in plasma with a precision of 8% (SD) at 50 pg ml-1, 22% (SD) at 20 pg ml-1 and a lower limit for quantitative determination of 10 pg ml-1. Plasma concentrations of clonidine In 10 subjects given a single 50μg oral dose are reported.
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    Mass spectral analysis of perfluoroacylated derivatives of some arylalkylamines of biological interest (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 441-449 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Numerous amines of biological interest can acetylated in aqueous solution, extracted and then perfluoroacylated for analysis by electron-capture gas chromatography. The structures of the products which are obtained can be confirmed by recording and interpreting their mass spectra. The electron impact mass spectral behaviour of various derivatized amines (amphetamine, ephedrine, p-hydroxyamphetamine, 3-methoxytyramine, norephedrine, normetanephrine, norpseudoephedrine, p-octopamine, 2-phenylethylamine, phenylethanolamine, pseudoephedrine, phentermine, m-tyramine and p-tyramine) is described.
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    Mass spectral identification of benzothiazole derivatives leached into injections by disposable syringes (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 450-454 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Five benzothiazole derivatives leached into injections by the rubber plunger-seals of disposable syringes were identified by electron impact (EI) and chemical ionization (CI) mass spectrometry. These are 2-hydroxybenzothiazole, 2-mercaptobenzothiazole, 2-(methylmercaptopto)benzothiazole, 2-(2-hydroxyethoxy)benzothiazole and 2-(2-hydroxyethylmercapto)benzothiazole. 2-Mercaptobenzothiazole is used as a vulcanization accelerator. The other four compounds are formed from the zinc derivative of 2-mercaptobenzothiazole during sterilization with ethylene oxide. Toxicological, technological and legal consequences of the leaching are discussed briefly.
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    Positive and electron capture negative ion methane chemical ionization mass spectrometry of pyrrolizidine alkaloids (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 455-461 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pulsed positive and negative ion methane chemical ionization mass spectrometry of pyrrolizidine alkaloids is reported. Positive ion spectra are characterized by a high relative abundance of [MH]+ ions while the negative ion spectra exhibit ion peaks due to dissociative electron capture. Fragmentation in both positive and negative ion spectra primarily occurs at the ester groups with the positive charge residing with the pyrrolizidine ring system while the negative charge in contrast tends to reside with the necic acid moiety. Esterification at C-9 v. C-7 can be distinguished for non-cyclic esters of retronecine in the positive ion specta.
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    URL: http://dx.doi.org/10.1002/bms.1200110904
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    Determination of phenobarbital, p-hydroxy-phenobarbital and phenobarbital-N-glucoside in urine by gas chromatography chemical ionization mass spectrometry (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 462-465 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A sensitive and efficient analytical procedure was developed to determine phenobarbital-N-glucoside, phenobarbital and p-hydroxyphenobarbital in urine. The stable-isotope labeled internal standards used in this assay were obtained in urine from a subject who ingested 15N-labeled phenobarbital.
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    URL: http://dx.doi.org/10.1002/bms.1200110905
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    Comparison of two methods for determining intramolecular 13C/12C ratios of acetic acid (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 472-474 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 13C/12C ratios of the carboxyl and methyl carbons of acetic acid were determined by two published methods, using the thermal decomposition of sodium acetate and calcium acetate respectively. Comparison of the results obtained on a variety of samples revealed a systematic disagreement of 4.0% between the two methods. The source of this discrepancy is shown to be a fractionation associated with the calcium acetate method.
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    URL: http://dx.doi.org/10.1002/bms.1200110907
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    High-performance liquid chromatographic isolation and fast atom bombardment mass spectrometric identification of di-N-desethylamiodarone, a new metabolite of amiodarone in the dog (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 466-471 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Amiodarone is an antiarrhythmic drug which has received considerable attention in recent years. It has been suggested that the unusual pharmacodynamic characteristics of this drug may be due in part to the influence of active metabolites. Using fast atom bombardment (FAB) mass spectrometry we have identified a new metabolite of amiodarone, the di-N-desethyl analog (DDEA). This metabolite was present in the blood of dogs treated with the parent drug, and showed a greater affinity for myocardium than did the parent drug. The unique features of FAB mass spectrometry over electron impact mass spectrometry was an essential element in facilitating the identification of this new metabolite. Whether or not this metabolite has pharmacologic activity or is responsible for some of the side effects occurring during amiodarone administration is not known.
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    A gas chromatographic/mass spectrometric assay for flutroline, a γ-carboline antipsychotic agent, with direct derivatization on a moving needle injector (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 482-485 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method has been developed for the determination of flutroline in plasma using capillary gas chromatography and selected ion monitoring detection of the TMS derivative. The method is linear over the concentration range of 3-60 ng ml-1 and was used to define the drug pharmacokinetics and bioavailability in animals and man. A novel method for direct derivatization on the tip of a moving needle injector is described.
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    URL: http://dx.doi.org/10.1002/bms.1200110909
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