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  • 1
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A tandem mass spectrometric method is described which allows the assignment of stereochemistry to fragment ions comprising intact sugar subunits of larger glycosides without chemical degradation and product isolation by chromatography. The approach relies on the mass selection of the ‘sugar ion’ of interest followed by analysis of stereoselective fragmentation induced by low-energy collisional activation. The daughter ion spectra provide configurational fingerprints of the selected sugar ions which can be matched for identity with reference spectra obtained from suitable precursors of known stereochemistry. Glucose, mannose and galactose furnished the required set of the most important reference ions. By using peracetyl (and perdeuterioacetyl) derivatives, galactose was readily identified as the glycosidic sugar constituent of the (known) antibiotic papulacandin B and a further (unknown) congener.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 329-332 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Deactivation ; Polymethylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 469-474 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Packed capillary columns ; On-Line multidimensional chromatography ; Gas chromatography, GC ; Capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The introduction of selected fractions from a liquid chromatograph into a gas chromatograph has been described; however, analyses were performed by off-line experiments requiring collection and reinjection of the separate fractions or by on-line procedures where disadvantageously, only a fraction of the separated peak or a well resolved component in a mixture could be introduced into a gas chromatograph. This disadvantage is overcome by the apparatus and method described in this paper, which utilizes a multidimensional chromatography system employing a high efficiency, packed capillary LC column coupled on-line to a capillary gas chromatograph.The liquid chromatograph (so designed) can act as a highly efficient clean-up or chemical class fractionation step prior to introduction into the gas chromatograph, significantly reducing sample preparation times in many applications. Thus minor components in a complex matrix can be determined without prior sample clean-up, an example of which is the determination of polychlorinated biphenyls in a complex hydrocarbon matrix.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 29-32 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography ; Injection techniques ; Reproducibility ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analysis of the precision obtained using commercially available microvalve injectors is reported for three modes of injection: conventional split; timed-split; and direct. Results from this study show that good precision (〈 3% RSD for external standard and 〈 1% RSD for internal standard methods) can be obtained with capillary supercritical fluid chromatography (SFC). However, particular attention must be paid to the type of valve used, the orientation of the column relative to the valve, the mode of interfacing or connecting the column to the valve, and the type of pressure or density programming used for the analysis as all of these factors will affect the reproducibility.
    Additional Material: 1 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. 65-69 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Temperature/pressure programming ; Density/temperature programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The theoretical and practical implications of simultaneous temperature/pressure and synchronized density/temperature programming are considered. Examples are shown for separations of dimethylpolysiloxanes where these techniques provide superior separation over their analogous isothermal programming methods.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0935-6304
    Keywords: GC/MS, high temperature ; Interface, high temperature ; Capillary columns, glass ; OH-terminated polysiloxane, OV-225-OH ; Immobilization by condensation ; Crosslinker, cyanopropyltriethoxysilane ; Analysis of free bases and metallo-petropophyrins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This contribution describes GC/MS analysis of natural petroporphyrin extracts containing alkylporphyrins either as vanadyl complexes or as demetalated free bases. The combination of high temperature glass capillary gas chromatography with mass spectrometry allows, for the first time, direct determination of electron impact mass spectra of separated alkylporphyrins, making additional purification and derivatization unnecessary. The separation is carried out on glass capillary columns coated with the high temperature-stable medium polar, OH-terminated, polysiloxane phases PS 086 and OV-225-OH. The paper gives detailed working directions for the preparation of the high temperature GC/MS-interface, and of the high temperature stable OV-225-OH columns (max. working temperature 390°C).
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 548-554 
    ISSN: 0935-6304
    Keywords: Gas liquid chromatography (GLC) ; Fused silica capillary columns ; Alkali flame ionization detection (AFID) ; Mass spectrometry (MS) ; Quantitation in human serum ; Ethylenediamine ; Aminophylline ; Small molecular weight amines and diamines ; m-Toluoyl derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A specific and sensitive method for the determination of ethylenediamine in human plasma is described. The aqueous sample is treated with m-toluoyl chloride, yielding the N,N′-bis(m-toluoyl) derivative of the diamine, which is extracted into dichloromethane and quantitated after “on column” methylation by capillary gas liquid chromatography with alkali flame ionization detection. The corresponding derivative of putrescine serves as internal standard. The assay is reproducible and calibration curves are linear over the concentration range 0.05 to 10 μg · ml-1. The lower detection limit is about 10 ng · ml-1. The structures of the compounds of interest eluting from the capillary column are examined by gas liquid chromatography/mass spectrometry. The assay has been applied to the analysis of ethylenediamine in plasma following the administration of aminophylline and ethylenediamine in a cross-over study to patients with bronchopulmonary diseases. The method also proves suitable for measuring other primary and secondary amines and diamines in aqueous solutions by gas liquid chromatography.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 446-448 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Fused silica capillaries ; Packed capillary columns ; Porous ceramic bed supports ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Porous ceramic bed supports for fused silica packed capillary columns utilized in liquid chromatography were prepared by polymerizing solutions containing potassium silicate in-situ within a column to create a mechanically stable, rugged, and easily constructed termination. The effect of the bed support length on efficiency, and comparisons to glass wool bed supports, were considered in terms of column efficiencies and hydrodynamic variables. Results obtained indicate better performance for the ceramic bed support.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 477-478 
    ISSN: 0935-6304
    Keywords: Capillary SFC ; Reproducibility ; Pump filling method ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 13-18 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Biphenyl polysiloxane ; Stationary phase ; Polarizable phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A crosslinkable biphenylmethylpolysiloxane stationary phase was synthesized for capillary column gas chromatography and compared with methyl, phenyl, and cyanopropyl polysiloxane stationary phases for the separation of isomeric polycyclic aromatic compounds. While the new phase gave similar separations of nonpolar isomers when compared to the nonpolar phases, separations of polar isomers were greatly improved because of the induced polarity of the biphenyl group of the stationary phase by the solute molecules. This polarizable stationary phase offers a unique selectivity which is not available in other stationary phases.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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