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  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 295-299 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 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. 276-278 
    ISSN: 0935-6304
    Keywords: HPLC, Packed microbore columns ; Band broadening and flow rate ; Calculated van Deemter plot ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 411-414 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Automated derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the gas chromatographic analysis of complex biological samples, the most time-consuming and error-prone steps are the pretreatment required for isolation and purification of the compounds of interest and, for most analytes, the derivatization to chemically and thermally stable compounds with high volatility. These wet-chemical steps are usually carried out manually, and for routine analysis of large numbers of samples they are often rate-limiting. A dedicated automated derivatizer has been constructed, the employment of which significantly reduces the time required for manual labor and increases the reproducibility of derivatization and hence the accuracy of analysis.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 709-714 
    ISSN: 0935-6304
    Keywords: Deactivation ; Capillary columns ; Silylation ; HPLC-silica ; Surface group concentration ; Pore alterations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-temperature silylation (HTS) used for the deactivation of capillary columns was studied on the silica commonly used in HPLC to gain a better insight into this process. LiChrosorb Si 100 was silylated with disilazanes at different temperatures and the materials obtained were compared in terms of organic and silanol group surface concentration, IR reflection spectra, HPLC behavior, and pore distribution parameters. Applying diphenyltetramethyldisilazane, the volatile reaction products were monitored during the HTS process. With increasing silylation temperature up to 400°C the silanol surface concentration is reduced to a very small level independent of the organic group concentration which exhibits a broad maximum depending upon substituents and temperature. Up to 350°C triorganosiloxy groups prevail as bonded organic groups. It could be proved that HTS is accompanied by pore alterations of the silica matrix. Arguments proposed by different authors in explaining HTS effects are discussed.
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 220-221 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Packed microbore capillaries ; Miniaturization of components ; Estimation of dead volumes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 662-666 
    ISSN: 0935-6304
    Keywords: Capillary GC ; GC/MS ; Reducing sugars ; NPD ; Derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reduction of sugar methoximes with sodium cyanoborohydride followed by permethylation with CH3SOCH2-/ICH3 affords the corresponding deoxy(methylmethoxylamino)alditol O-methyl ethers, which are amenable to capillary gas chromatography. Derivatization proceeds under mild conditions with high yields. Only a single derivative is formed for each reducing sugar. All aldose derivatives can be separated in a single chromatographic run on glass capillaries coated with Carbowax 20 M or Superox 0.1. Good linearity was found. The introduction of the nitrogen atom in the sugar molecule makes these derivatives suitable for selective detection by the NPD. The El-mass spectra contain intense characteristics ions at m/z 74 for aldoses and at m/z 280 for reducing disaccharides, together with a (M - 15)+ion. These fragments are very suitable for highly sensitive GC-MS analysis by selective single ion monitoring.
    Additional Material: 5 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 433-433 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 429-429 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 787-792 
    ISSN: 0935-6304
    Keywords: Chiral gas chromatography ; Microbore capillaries ; Enantioselectivity ; Chiral polysiloxane, crosslinking ; Chirasil-Val ; Selector, chiral ; Thermal stability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermal stability and enantioselectivity of chiral polysiloxane stationary phases for gas chromatography depend upon the composition and purity of the polymer matrix, its functional groups, the chiral selector, and the pretreatment of the inner surface of the capillary. Under proper conditions, narrow-bore capillaries can be prepared which may be used up to 300 °C for short times. Crosslinking of the phases is achieved by heating.
    Additional Material: 6 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 2 (1975), S. 254-260 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The extent of C-methylation, an artifact of the permethylation procedure used to derivatize peptides for mass spectrometric sequencing, was investigated by mass spectrometry. Ten glycine-containing peptides were N-acetylated and then permethylated by the Hakomori method and analyzed by chemical ionization and, in some cases, by electron ionization mass spectrometry. A comparative study was made of the tripeptides Gly Pro Ala and Ala Pro Gly, derivatized by three permethylation procedures. The results show that while C-methylation occurs primarily at glycine, other amino acids (Gln, Glu, Met, Tyr) are also C-methylated, but to a lesser degree. The extent to which C-methylation occurs varies widely and depends on residue position and on the identity of neighboring residues. Such artifacts could lead to serious errors in peptide sequences determined by mass spectrometry, especially when mixtures of peptides are analyzed.
    Additional Material: 4 Tab.
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