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Title: Studies of atmospheric pressure ionisation mass spectrometry in countercurrent chromatographic analysis of polar small molecules
Author: Jones, J. J.
Awarding Body: University of Wales Swansea
Current Institution: Swansea University
Date of Award: 2004
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In this thesis, the initial use of API-MS in CCC was demonstrated with the analysis of polar herbicides by CCC/ESI-MS including MS/MS fragmentation by collision-induced dissociation (CID). This study highlighted the traditional problems commonly associated with CCC/MS methodologies such as high backpressure and CCC coil failure. Six benzodiazepines were analysed by CCC/ESI-MS performed on two countercurrent chromatographs, demonstrating the advantages of small coil volumes in rapid CCC analysis. It was determined that for these compounds, modification of the mobile phase stream by addition of a dilute organic acid greatly increased signal responses under CCC/ESI-MS. Comparative studies were performed on LC/ESI-MS and compound structural information was successfully collected from both techniques. The development of a new solvent system consisting of butyronitrile:acetonitrile:water was demonstrated for the analysis of hydrophilic compounds by CCC and CCC/MS, as an alternative to the n-butanol:water based solvent systems. The successful employment of this system was shown in both reverse and normal phase CCC modes, in the study of stimulants and barbiturates by CCC/MS and LC/MS. Both ESI and APCI ionisation methods were employed in these studies, and this thesis presents the first known applications of APCI in CCC. The newly developed butyronitrile:acetonitrile:water solvent system was then further employed in the study of zwitterionic sulfobetaine surfactants by CCC/ESI-MS. The application of a small coil volume CCC instrument and the butyronitrile:acetonitrile:water based solvent systems was able to provide convenient analysis times of less than one hour for very hydrophilic substances, with the addition of mass spectrometry as a highly selective detection method.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available