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  • 1
    ISSN: 1612-1112
    Keywords: Column liquid Chromatography ; Chemiluminescence detection ; Solid reagent bed ; Quinone detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The combination of solid-state peroxyoxalate chemiluminescence detection and post-column chemical reaction systems in liquid chromatography is investigated. Bis-2,4,6-trichlorophenyloxalate (TCPO) is added from a solid reagent bed with the fluorophore, 3-aminofluoranthene, immobilized on glass beads. Hydrogen peroxide generated photochemically by quinone analytes is measured. Flow splitting is shown to be a simple means of reagent addition with a negligible band broadening effect. This system is compared to a more flexible dualpump design. To minimize band broadening in both systems, the reagent bed is located out of the path of the chromatographic effluent. Detection limits are in the sub-picomole range, an imporvement relative to those previously reported with TCPO added in the liquid phase. These systems can be easily be adapted for detection of peroxide generated by other post-column reactions.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; On-line LC-CE ; Sample pretreatment ; Matrix effects ; Benzoic acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various methods are currently under investigation to improve concentration detection limits in capillary electrophoresis (CE). Stacking and isotachophoresis coupled in-line with free-solution electrophoresis are the techniques most frequently used. Samples containing a high and/or varying salt concentration, such as urine and serum, are difficult to handle: usually a significant loss in electrophoretic efficiency is observed compared with samples possessing a low electric conductivity. In the present paper an alternative approach is developed, i.e. a liquid chromatographic (LC)-type of sample pretreatment is coupled on-line with CE. To demonstrate the feasibility of this approach, the separation of three model compounds (benzoates) in water containing up to 400 mM of sodium chloride is studied using a 50 mM borate CE buffer of pH 9.5. The direct injection of samples with high salt concentrations in CE results in peak splitting and/or serious band broadening. These problems are not encountered when using the present LC-CE system. In addition, the detection limits are hardly influenced by the salt concentration of the sample; this underlines the robustness of the system.
    Type of Medium: Electronic Resource
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