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  • 1
    ISSN: 0935-6304
    Keywords: Coupling LC/GC ; Retention gap ; Polychlorinated biphenyls ; Sediment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Narrow-bore column liquid chromatography coupled on-line with capillary gas chromatography (LC/GC) is used for the determination of polychlorinated biphenyls (PCBs) in sediment via a heart-cutting technique. This method is compared with a method in which two off-line column clean-up steps are used with subsequent analysis by capillary gas chromatography. For the LC/GC analysis the recovery of PCBs was 90-100%. For two sediment samples from the river Meuse the LC/GC and the other, more laborious method showed good agreement.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0935-6304
    Keywords: Polar solvents ; Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coupling column liquid chromatography and gas chromatography on-line is becoming more important in analytical chemistry. Especially when large amounts of polar solvents can be introduced into the gas chromatograph without any problem, the technique will offer new possibilities. With a DPTMDS retention gap, evaporation rates and flooded zones of some solvents have been determined. Two modes of operation using partially concurrent solvent evaporation conditions are discussed: (1) injecting a sample via a loop of an LC valve followed by introduction into the gas chromatograph with an LC pump; (2) trace enrichment on a precolumn followed by on-line desorption with n-propanol into the gas chromatograph. Preliminary results for a splitter system, inserted between the retention gap and the analytical column which allows a considerable increase of the evaporation rate are also presented.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 793-796 
    ISSN: 0935-6304
    Keywords: Microcolumn liquid chromatography ; Flame photometric detection ; Organophosphorus compounds ; On-line preconcentration ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The potential of an interface for the on-line coupling of microcolumn liquid chromatography (LC)and a flame photometric detector (FPD) has been further investigated. With the micro-LC/FPD system, relatively high-molecular-weight polar compounds such as cyclic adenosine monophosphate, guanosine monophos- phate, glucose monophosphate, fructose monophosphate, and phytic acid were separated and selectively detected. In order to increase the sensitivity, on-line preconcentration with a microprecolumn inserted in the rotorof a Valcovalve has been applied. Preliminary results have shown that an injection volume of at least 500 1-11 water containing organophosphorus acids at a 5-50 ng/rnl concentration level is possible.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Journal of Bioluminescence and Chemiluminescence 13 (1998), S. 31-40 
    ISSN: 0884-3996
    Keywords: chemiluminescence ; 10-methyl-N-(sulphonyl)-9-acridinium carboxamide ; liquid chromatography ; derivatization ; carboxylic acids ; ibuprofen ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: The synthesis of a new acridinium sulphonylamide label for the liquid chromatographic determination of carboxylic acids is described. The label 10-methyl-N-(p-tolyl)-N-(p-iodoacetamidobenzenesulphonyl)-9-acridinium carboxamide iodide is synthesized from 9-acridinecarboxylic acid by a seven-step reaction. Ibuprofen, used as test compound, is coupled to the reactive iodoacetamide group of the label by means of an alkylation reaction in dry acetonitrile for 20 min at 50°C in the presence of 18-crown-6 and potassium carbonate as base catalyst. The reaction mixture is injected into a liquid chromatographic system with chemiluminescence detection. Separation is performed on a Zorbax C18 column with acetonitrile-water-tetrahydrofuran (39:57:4, v/v/v) containing 10 mmol/L TBABr and 0.035% H2O2 as the mobile phase at a flow rate of 1.0 ml/min. Chemiluminescence detection is achieved by the post-column addition of 200 mmol/L potassium hydroxide dissolved in methanol-water (1:1, v/v) at a flow rate of 20 μL/min. The detection limit (S/N = 3) of derivatized ibuprofen is 60 pg (3 pg injected). © 1998 John Wiley & Sons, Ltd.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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