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  • Analytical Chemistry and Spectroscopy  (3)
  • Gas chromatography  (3)
  • 1995-1999  (6)
  • 1
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Polychlorinated biphenyls ; Cod liver oil
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary By application of a chromatographic column filled with Supelclean ENVI-Carb/Celite and elution with three solvents of different polarity three PCB fractions were obtained. Fraction A contained poly-ortho PCBs, Fraction B mono-ortho PCBs, and Fraction C non-ortho PCBs. The Supelclean ENVI-Carb/Celite column was used in combination with a sample preparation procedure for pre-cleaning of acid-stable chlorinated hydrocarbons such as DDT and its metabolites, HCH isomers, and regulation-relevant PCB congeners. The method was optimized using standard solutions of 55 PCB congeners, 8 chlorinated pesticides and contaminated cod liver oil samples. The influence of traces of remaining matrix on the elution profile of the organochlorine compounds on Supelclean ENVI-Carb/Celite was observed. Quantitation was carried out by GC-ECD with fused silica capillary columns of different polarity.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Microwave extraction ; Sample clean-up ; Organochlorine compounds ; Blubber of marine mammals
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and effective method is described for the extraction of organochlorine compounds (PCB 153, PCB 138, PCB 180, p,p′-DDE, α-HCH, γ-HCH, ε-HCH and HCB) from seal blubber and pork fat withn-hexane using a microwave technique. Heating of the non-polarn-hexane was achieved using a microwave transformer. The lipid content of the samples obtained by this extraction was identical to that by Soxhlet extraction. After separation of sample matrix and organochlorines on a silica gel column the organochlorine compounds were determined by GC-ECD. The efficiency of the method was tested with 500 mg spiked fat, extracted using various numbers of extraction cycles. Recoveries of organochlorine compounds in grey seal blubber and spiked pork fat generally exceeded 90 %.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 643-646 
    ISSN: 0935-6304
    Keywords: Gas chromatography/Mass spectrometry ; Chiral GC ; Deuterium-labeled compounds ; Hexachlorocyclohexane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 30 (1995), S. 1562-1566 
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 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.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chiral stationary phases ; Enantioseparation ; Toxaphene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of the enantiomers of the compounds of technical toxaphene (CTTs) on heptakis(6-O-tert-butyldimethylsilyl-2,3-di-O-methyl)-β-cyclodextrin (β-TBDM) has been studied by gas chromatography with electron-capture detection (GC-ECD). Enantiomers of eight of the nine CTTs under investigation were separated on this chiral stationary phase. Separations of the enantioners of CTTs have hitherto been achieved ontert-butyldimethylsilylated β-cyclodextrin (β-BSCD). The chiral resolution values and separation factors of the CTTs on β-TBDM have been compared with those obtained on β-BSCD. Although several components coeluted, enantioselective determination of three CTTs was possible in an extract of seal blubber. For each CTT the first-eluting enantiomer was enantioenriched. Enantioselective accumulation of2-endo, 3-exo,5-endo,6-exo,-8,8,9,10-octachlorobornane (B8-1412) in biota has been established for the first time.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 85-93 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Modified cyclodextrin phases ; Chiral organochlorines ; Biological samples ; Enantiomeric ratios ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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