Graduate Thesis Or Dissertation

Ion-pair high pressure liquid chromatography techniques for the determination of quaternary ammonium compounds

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  • Quaternary Ammonium Compounds, Qams, are an important class of chemicals which present interesting challenges to analysts. This thesis reports results of investigations on uses of ion-pairing techniques for separations and detection of Qams. Special apparatus for post-column solvent extraction of liquid chromatographic eluates was developed as part of this work. Analyses for Qams were developed using ion-pair extraction techniques with bromophenol blue, anthraquinone sulfate and naphthyl sulfate as ion-pair extraction reagents. Bulk extraction experiments were executed to evaluate the dependance of the ion-pair reagent concentration on the extraction efficiency of Qam ion pairs. The pH dependance on extraction efficiency for gallamine triethiodide and decamethonium bromide, bromophenol blue ion pairs was also evaluated. A solvent segmented flow injection analysis system was designed and assembled for the rapid evaluation of ion-pair extraction efficiency of several different Qams with bromophenol blue as the ion-pair extraction reagent. Separations of Qams using ion-pair liquid chromatography were developed using reverse phase columns and both alkyl sulfonic acid and tetramethylammonium salts in the mobile phase as ion-pair liquid chromatography reagents. A continuous post-column solvent extraction system was developed for the detection of Qam bromophenol blue ion pairs with bromophenol blue being added directly to the mobile phase eluents. Both isochratic and gradient separations were developed for several Qams which have medical importance.
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