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  • 1
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Urea herbicides ; Catalytic hydrolysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Narrow-bore column liquid chromatography ; Post-column derivatization ; Solid-phase reactors ; Catalytic hydrolysis ; On-line trace enrichment ; Immobilized enzyme
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of solid-phase reactors for post-column derivatization in narrow-bore HPLC (1.0mm i.d. analytical columns) is evaluated. Two systems are described, viz. for the determination of N-methylcarbamate pesticides and for that of urea and ammonia. The solid-phase reactor is packed with a strong anion exchange resin and urease immobilized on silica, respectively, to effect the catalytic hydrolysis of the solutes eluting from the analytical column. In both systems, the hydrolysis product is reacted with o-phthalaldehyde followed by fluorescence monitoring. Analytical data are presented and band broadening from various parts of the reaction detector system is discussed. An on-line trace enrichment procedure via a micro precolumn is descried for the trace level determination of N-methylcaramates in surface water samples.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrodialytic sample treatment ; On-line coupling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An electrodialytic sample treatment method coupled on-line with high-performance liquid chromatography (EDIST-HPLC) is discussed in this paper. The performance of EDIST as a function of the donor-phase (sample solution) flow rate, the voltage applied over the electrodialysis block, and the time of dialysis has been studied using the basic drug ephedrine as a model compound. Enrichment of the analyte by a factor of 10–20 was possible. The determination of human plasma spiked with ephedrine is briefly discussed.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; On-line coupling ; Ion-exchange membrane ; Ion-pair reagent
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant in the membrane was tetrabutylammonium hydroxide dissolved in acetonitrile/water, which effects an anion-exchange of methanesulphonate ions for regenerant hydroxide ions. The efficiency of the exchange process was found to be 99.9%. This enabled the direct introduction of the LC eluent, free of ions and with the proper acetonitrile/water ratio, into the GC. The applicability of the on-line LC-micromembrane-GC system has been illustrated for the potential drug eltoprazine, which is quantitatively recovered with a coefficient of variation for standard solutions of 3% at the 150 μg/ml analyte level.
    Type of Medium: Electronic Resource
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