on-Line Liquid Chromatography/fast Atom Bombardment Mass Spectrometry
Stroh, Justin G.
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https://hdl.handle.net/2142/70356
Description
Title
on-Line Liquid Chromatography/fast Atom Bombardment Mass Spectrometry
Author(s)
Stroh, Justin G.
Issue Date
1986
Department of Study
Chemistry
Discipline
Chemistry
Degree Granting Institution
University of Illinois at Urbana-Champaign
Degree Name
Ph.D.
Degree Level
Dissertation
Keyword(s)
Chemistry, Analytical
Abstract
Directly coupled liquid chromatography/fast atom bombardment mass spectrometry (LC/FABMS) employing a moving belt interface was used to analyze a number of mixtures including the partial hydrolysis products obtained from antiamoebin I, zervamicins IIA and IIB, leucinostatins, trichorzianines, didemnins, and paulomycins A and B, as well as the single components intact antiamoebin I, CC-1014B, and glyceollin. Initial studies using LC/FABMS were performed in conjunction with a jet spray depositor, which yielded weak and unstable signals. Improvements in signal strength and stability were made by the development of the fritted contact depositor, usage of LC microbore technology, and belt conditioning.
The capabilities of the improved LC/FABMS system were investigated. Operation in the negative ion mode was demonstrated with a mixture of substituted phosphazenes. The upper mass limit for analysis involving peptides was determined to be slightly higher than 2000 amu. The interface was tested for use the silica gel columns and it was found that the LC/FABMS interface was extremely sensitive to column bleed of silica gel.
Finally, it was observed that the LC/FABMS interface produced more structurally significant fragment ions than solids probe FABMS as demonstrated by comparison of the two techniques using paulomycin A.
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