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Title: Investigation of combined separation-mass spectrometry for the analysis of pharmaceutical products
Author: Cheasty, A. G.
Awarding Body: University College of Swansea
Current Institution: Swansea University
Date of Award: 1995
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Mycotoxins, by definition are the secondary metabolites of moulds and are toxic to man and animal. It is important, within the fermentation industry, to monitor their production. Traditionally, gas chromatography and liquid chromatography have been applied to the analysis of these compounds. Unfortunately, drawbacks with respect to speed of analysis, selectivity and detection were encountered. To overcome this, methodologies, for the analysis of the triglyceride components of vegetable oils and mycotoxin standards, have been designed with state-of-the-art chromatographic (supercritical fluid chromatography), separation (capillary electrophoresis) and detection (mass spectrometry) techniques and reported herein. The application of capillary SFC to the analysis of several vegetable oils yielded a rapid and powerful screening method that allows for differentiation between various oils. The development of a packed SFC methodology for the analysis of mycotoxins, based on retention indices, failed due to the lack of column selectivity for the mycotoxins and the retention standards. Nevertheless, a fast, efficient separation of mycotoxins was obtained. MS detection via thermospray ionisation provided the specificity necessary for peak elucidation. HPLC/MS with thermospray, electrospray and particle beam ionisation was applied to the analysis of the mycotoxins. Particle beam with electron ionisation and thermospray were found to be universal ionisation methods. Whilst the former yielded structural information, sensitivity was poor due to poor transport properties of this interface. Electrospray provided the best sensitivity. With capillary electrophoresis, MECC was required to enable the separation of both the neutral and ionic mycotoxins. Unfortunately, the use of non-volatile buffers and surfactants rendered this methodology unsuitable for coupling to the mass spectrometer.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available