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  • Analytical Chemistry and Spectroscopy  (3)
  • 1995-1999  (3)
  • 1
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 85-93 
    ISSN: 0935-6304
    Schlagwort(e): Capillary gas chromatography ; Modified cyclodextrin phases ; Chiral organochlorines ; Biological samples ; Enantiomeric ratios ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Four chiral stationary phases containing modified cyclodextrines diluted in or chemically bonded to a non-chiral phase were used to resolve chiral organochlorine compounds such as α-hexachlorocyclohexane (α-HCH), perdeuterated α-HCH (α-PDHCH), β-and γ-pentachlorocyclohexene (PCCH), oxychlordane, cis-and trans-chlor- dane, cis- and trans-heptachlorepoxide, PCB 95, PCB 132, PCB 149, and Chiral tozaphenes.The elution order was determined by analyzing standards with known enantiomeric excesses.Furthermore, an internal standard was used to even out slight variations in the ratio of peak hights of enantiomers which were determined from injection to injection.None of the chiral stationary phases resolved all chiral organochlorine compounds. However, the β-TBDM(35% heptakis (6-O-t-butyldimethylsilyl-2,3-di-O-methyl)-β-cyclodextrin in OV 1701) column allowed the separation of all compounds under investigation except for PCB 95 and chiral toxaphenes.Emphasis was placed on the separation of as many as possible enantiomers on a chiral phase by application of one temperature program and with respect to unambiguous quantitation of biological samples such as bludder and liver of marine and terrestrial mammals.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
    Standort Signatur Einschränkungen Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 643-646 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography/Mass spectrometry ; Chiral GC ; Deuterium-labeled compounds ; Hexachlorocyclohexane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Perdeuterated α-1,2,3,4,5,6-hexachlorocyclohexane (α-PDHCH) was synthesized and isolated in pure form. α-PDHCH was baseline separated from unlabeled α-HCH by high resolution gas chromatography on different stationary phases. α-PDHCH was also resolved into its enantiomeric forms by application of a chiral GC phase. Furthermore, chiral chromatography of a mixture of labeled α-PDHDH and unlabeled α-HCH resulted in four peaks. Standard solutions of α-PDHCH are recommended both as recovery standard for sample clean-up and as internal standard for the quantitation of chlorinated hydrocarbons with GC/MS or GC/ECD in environmental samples.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Standort Signatur Einschränkungen Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 30 (1995), S. 1562-1566 
    ISSN: 1076-5174
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: A simple and rapid method for counting the number of internal disulfide bridges in a protein by incubation with 2-mercaptoethanol and electrospray mass spectrometry analysis of the products was developed. 2-Mercaptoethanol yields intermediate mixed disulfides during reduction of a protein. This results in a molecular weight increase of the protein by 78 Da per disulfide bond, which can easily be determined by electrospray mass spectrometry (ESMS). The number of mercaptoethanol adducts observed by ESMS reveals the number of disulfide bridges in the peptide or protein. Since the protein-mercaptoethanol-disulfide bonds are themselves further reduced by excess mercaptoethanol, the course of the reaction has to be followed in order to detect the maximum number of intermediates. Owing to the volatility of mercaptoethanol, samples can be taken out of the reaction solution for MS analysis without prior purification. Successful experiments were carried out using proteins with one, two, four or six S—S-bonds, covering a mass range from about 1 to over 23 kDa.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
    Standort Signatur Einschränkungen Verfügbarkeit
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