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  • 1
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 685-691 
    ISSN: 0935-6304
    Schlagwort(e): On-line LC-GC-MS ; PCBs ; Non-ortho CBs ; Human blood plasma ; Dinitroanilinopropyl modified silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method for the determination of non-, mono- and di-ortho substituted polychlorinated biphenyls in human blood plasma is presented. The non-ortho CBs are isolated from the bulk of PCBs by HPLC on a dinitroanilino-propyl silica column and collected as a heart-cut fraction that is transferred on-line to GC-MS utilizing concurrent solvent evaporation technique. The on-line coupling serves to lower the limit of determination and to partly automate the sample clean-up. The di- and mono-ortho CBs are analyzed by off-line GC-ECD using two different columns. Sample pre-treatment is performed by extraction with organic solvents and fractionation on silica gel. A high reproducibility and an absolute over-all recovery of approximately 70 % is demonstrated. The method is applied to samples of blood from 5 individuals. All the samples demonstrated a similar relative concentration profile. It was also shown that three CB congeners (CB 126, CB 156 and CB 170) contributed to the major part of the toxic equivalent quantity of the PCB content in the blood.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 605-616 
    ISSN: 1040-7685
    Schlagwort(e): GC-AED ; optimization of response ; PCBs ; methylsulfonyl-PCBs ; biological samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Gas chromatography-atomic emission detection (GC-AED) has been evaluated in order to determine the optimal conditions for chlorine and sulfur response of chlorinated biphenyls (CBs) and methylsulfonyl metabolites of CBs (MeSO2-CBs). The influence of the shape of the capillary column end facing the plasma, make-up gas flow, additional transfer line make-up gas flow and reagent gas flows on the detector response has been studied. Using an additional make-up gas flow applied through a transfer line capillary having a decreased outlet diameter yielded an increased detector response with minimum detectable levels for sulfur and chlorine of 1.7 and 20 pg, respectively. Further, a substantial decrease in peak tailing was achieved. The applicability of the method for analysis of biological materials is demonstrated by the determination of the main CB congeners present in human blood and of MeSO2-CBs in seal blubber.
    Zusätzliches Material: 11 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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