Use this URL to cite or link to this record in EThOS:
Title: Studies of supercritical fluid chromatography atmospheric pressure ionisation mass spectrometry
Author: McCullagh, M. A.
Awarding Body: University of Wales Swansea
Current Institution: Swansea University
Date of Award: 1999
Availability of Full Text:
Access from EThOS:
The advantages of packed column supercritical fluid chromatography (SFC) over LC in terms of speed of analysis, increased efficiency and speed of method development have been shown to be of particular use for chiral separations of β-Blockers, where UV detection was employed. Interfaces that enabled SFC-MS to be effected were initially reviewed to enable the development of an interface to couple an HP G1205 A supercritical fluid chromatograph to the APCI source of the Finnigan TSQ 700 and LCQ ion trap. Effectively, SFC-MS has been effected with a pre-expansion split and a post-expansion interface thus allowing a portion of the eluent to enter the ionisation region of the mass spectrometer from the supercritical fluid chromatograph. For the work presented, approximately twenty five per cent of the eluent entered the ionisation source. Later, SFC was coupled with the ES ionisation source of the LCQ ion trap. The interfaces developed offer enhanced specificity of identification, with improved detection limits over UV and allowed a comparison of effecting SFC-API-MS with the two mass spectrometers. Being able to facilitate SFC-ES-MS and SFC-APCI-MS with an LCQ ion trap allowed a comparison of the ionisation techniques for the analytes of interest. The differences in effecting SFC-API-MS-MS with the LCQ ion trap and the SQ 700 were illustrated. Anti cancer agents are of great interest to the pharmaceutical industry. Two of synthetically produced groups of lignans were analysed using SFC-APCI-MSn and SFC-ES-MSn. Acceptable resolution of the enantiomers and low detection limits are shown, thus showing SFC-API-MS to be a potential tool to help solve chiral analysis problems within industry. Investigations in the use of a Shandon hypercarb column to effect packed column SFC-API-MS have also been explored. Packed column SFC-API-MSn is shown for benzodiazepines, sulphonamides and carbamate pesticides. Fast analysis times, acceptable resolution and low detection limits for the three classes of compounds are shown.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available