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  • 1
    Electronic Resource
    Electronic Resource
    On-line dialysis solid-phase extraction coupled to capillary electrophoresis (1998)
    Weinheim : Wiley-Blackwell
    Electrophoresis 19 (1998), S. 2944-2949 
    Details
    ISSN: 0173-0835
    Keywords: Capillary electrophoresis ; Dialysis ; Sample pretreatment ; Serum ; Sulfonamides ; Urine ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: A fully automated dialysis solid-phase extraction (SPE) sample preparation procedure is coupled on-line to capillary electrophoresis (CE) for the first time. The system is used to determine sulfonamides in serum and urine. The dialysis unit serves to remove proteins and particulate matter. Reconcentration of the analytes is performed with a small SPE column while (in)organic salts and other interferences are removed simultaneously. Finally, the analytes are desorbed and injected, via a homemade interface, into the CE system. Limits of detection (LOD) of 0.05-0.1 and 0.05-0.3 μg/mL are obtained in urine and serum, respectively. The within-day and between-day precisions are in the range of 2-6% and 3-8%, respectively, for a concentration of five times the LOD. The dialysis SPE-CE system was used over a period of six months for the analysis of over 500 serum and urine samples without problems such as clogging of the CE capillary or SPE column.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/elps.1150191625
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  • 2
    Electronic Resource
    Electronic Resource
    Analyte identification in capillary electrophoretic separation techniques (1998)
    Weinheim : Wiley-Blackwell
    Electrophoresis 19 (1998), S. 2753-2776 
    Details
    ISSN: 0173-0835
    Keywords: Capillary electrophoresis ; Capillary electrochromatography ; Analyte identification ; Spectrometric detection ; Review ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: A review on applications of on-line hyphenation in capillary electrophoresis and capillary electrochromatography for the identification of migrating analytes is presented. There is an urgent need for unambiguous analyte identification by combining spectral information and observed migration times, because the parameters influencing the migration times and separation efficiencies in these separation techniques are not easily controlled, especially when real samples containing unknown interferences have to be analyzed. The spectrometric techniques covered here are ultraviolet and visible radiation (UV/Vis) absorption, fluorescence including fluorescence line-narrowing spectroscopy, Raman spectroscopy, nuclear magnetic resonance and mass spectrometry. Attention is essentially confined to literature reports in which the extra information provided by the detector is really used for identification purposes, especially in real-life samples, while the interfacing as such and analyte detectabilities in standard solutions are only briefly discussed. This article covers an extensive fraction of the literature published on this topic until the beginning of 1998.
    Additional Material: 18 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/elps.1150191604
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  • 3
    Electronic Resource
    Electronic Resource
    An acridinium sulphonylamide as a new chemiluminescent label for the determination of carboxylic acids in liquid chromatography (1998)
    New York : Wiley-Blackwell
    Journal of Bioluminescence and Chemiluminescence 13 (1998), S. 31-40 
    Details
    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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