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  • Analytical Chemistry and Spectroscopy  (7)
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  • 1
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 5 (1991), S. 484-490 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The direct coupling of capillary electrophoresis (CE) and mass spectrometry, combined with ionspray ionization using a coaxial capillary arrangement, is described. The CE/mass spectrometer interface is shown to be effective for the analysis of native and tryptic peptides and of proteins of high molecular weight such as bovine serum apotransferrin ( ≈78kDa). Adsorption of cationic analytes under acidic buffer conditions is minimized through the use of a non-covalent coated capillary possessing an overall positive charge. Since the direction of the electroosmotic flow is thus reversed, compared to that in conventional CE separation on uncoated capillaries, migration of cations is achieved by applying a negative voltage (typically - 30kV) at the injector end of the capillary. In addition to the inherent advantage of providing pre-formed cationic species for mass spectral detection, this arrangement permits analysis of proteins of high isoelectric points even at low pH. The ability to conduct electrophoesis of globular proteins under acidic conditions also provides a means of monitoring their conformational changes, as reflected both by the variation of migration times and by concurrent changes in the multiply charged ion envelopes.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The development of microbore packet-column supercritical fluid chromatography/atmospheric pressure chemical ionization mass spectrometry (SFC/APCI-MS) for the analysis of polycyclic aromatic compounds (PAC) is described. The SFC system was coupled to the mass spectrometer using an improved interface designed to accommodate commercially available fused silica restrictors. The atmospheric pressure chemical ionization characteristics of PAC are discussed and the use of chemical ionization reagents to modify the type of spectra obtained is described. With selected-ion monitoring techniques the interface provided detection limits in the low picogram range for individual PAC standards. Using a photoionization detector for the off-line optimization of chromatographic conditions, SFC/APCI-MS was applied to the analysis of complex mixtures of PAC in coal tar and tar sand oil extracts. Tandem mass spectrometry was used to provide structural information.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 5 (1991), S. 307-308 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Ionspray mass spectrometry has been used to monitor the purification of saxitoxin, the parent compound in the family of toxins responsible for paralytic shellfish poisoning (PSP), from a strain of the dinoflagellate Alexandrium excavatum. Quantitative results obtained by flow-injection analysis are compared to those obtained by high-performance liquid chromatography with post-column oxidation and fluorescence detection. The coupling of liquid chromatography and capillary electrophoresis with ionspray mass spectrometry is described for the separation of mixtures of PSP toxins and the highly potent pufferfish toxin tetrodotoxin. Tandem mass spectrometry is used to provide the structural information, and the ability to distinguish isomeric PSP toxins both chromatographically and mass spectrometrically is demonstrated.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 61-64 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography/Mass spectrometry ; Packed column ; Capillary column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A frit restrictor interface for capillary column supercritical fluid chromatography/mass spectrometry (SFC/MS) has been constructed and used for the analysis of high boiling point alkanes. Packed column SFC/MS is described using both a moving belt liquid chromatographic/mass spectrometric interface and a thermospray source in the filament-on mode.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A combined liquid chromatography/mass spectrometry (LC/MS) method using ion-spray ionization is described for the sensitive determination of okadaic acid and dinophysistoxin-1, the principal toxins implicated in cases of diarrhetic shellfish poisoning. The method is used to confirm the presence of okadaic acid in a culture of the dinoflagellate species Prorocentrum concavum and in natural populations of dinoflagellates from eastern Canadian waters. Several analogues of the toxin have also been detected. Quantitative results are comparable to those obtained by high performance liquid chromatography with fluorescence detection. With slight modifications, the LC/MS method is also used to analyse the fluorescent anthrylmethyl ester of okadaic acid. Preliminary tandem mass spectrometric results, obtained using fast-atom bombardment ionization, are presented for okadaic acid.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 27 (1992), S. 660-666 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass calibration for ion spray mass spectrometry can be achieved by using cluster ions formed by flow injection of solutions of alkali metal salts in aqueous acetonitrile into the liquid flowing to the ion spray needle. Source contamination is thereby reduced to a minimum. For quadrupole mass analyzers, sodium iodide provides an ideal compromise between undesirable spectral complexity and spacings between calibrant mass peaks sufficiently close that interpolation errors are negligible. When much closer spacings are required, protonated water clusters provide an excellent calibration up to about m/z 1000. If higher mass ranges are required with a large number of calibrant peaks, a solution of mixed alkali metal iodides does provide the expected spectra but intensities are poor at higher m/z values. For liquid chromatography with on-line mass spectrometry (LC/MS) the mass calibration may be checked without changing the mobile phase by post-column flow injection of a cesium carbonate solution, since the carbonate anion is wholly displaced by the anion of the mobile phase acid modifier, resulting in no mixed clusters. The metal salt calibrants have the additional advantage of being useful over a wide range of tuning parameters in the atmospheric pressure ionization source, covering those appropriate to both relative molecular mass determinations of large proteins and to LC/MS of small analyte species.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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