Chromatographic separations of enantiomers and underivatized oligosaccharides

dc.contributor.advisor Daniel W. Armstrong Liu, Ying
dc.contributor.department Chemistry
dc.contributor.other Chemistry 2018-08-24T18:38:33.000 2020-06-30T07:15:52Z 2020-06-30T07:15:52Z 2004-01-01
dc.description.abstract <p>My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS).;Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC.;Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence.;LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic resolution, high column stability, and high sensitivity. In addition, this method showed potential usefulness for the sensitive and quick analysis of hydrolysis products of polysaccharides, and for trace level analysis of individual oligosaccharides or oligosaccharide isomers from biological systems.</p>
dc.format.mimetype application/pdf
dc.identifier archive/
dc.identifier.articleid 2179
dc.identifier.contextkey 6090710
dc.identifier.s3bucket isulib-bepress-aws-west
dc.identifier.submissionpath rtd/1180
dc.source.bitstream archive/|||Fri Jan 14 18:58:56 UTC 2022
dc.subject Chemistry
dc.subject Analytical chemistry
dc.title Chromatographic separations of enantiomers and underivatized oligosaccharides
dc.type dissertation
dspace.entity.type Publication
relation.isOrgUnitOfPublication 42864f6e-7a3d-4be3-8b5a-0ae3c3830a11 Doctor of Philosophy
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