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Title: Analysis of pharmaceutical products and nucleotides by LC-MS and tandem mass spectrometry
Author: Marques Pereira, M. L.
Awarding Body: University of Wales Swansea
Current Institution: Swansea University
Date of Award: 1999
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Tandem mass spectrometry and chromatographic techniques coupled with mass spectrometry are demonstrated to be extremely useful in independent investigations of biochemical and pharmacological compounds. The first chapter gives some insight into the theory behind the chromatographic and mass spectrometric techniques used. Cyclic nucleotides are vital components in biochemical signal transduction and regulation, and thus the enzymes which regulate their intracellular levels are of great interest as pharmacological targets. In chapter 2, fast atom bombardment - collision induced dissociation and mass analysed ion kinetic energy spectrometry is compared with electrospray - tandem mass spectrometry, in a quadrupole ion trap, for the structural characterisation of cyclic nucleotides and cyclic nucleotide analogues. These are used as site selective activators of cyclic nucleotide - dependent protein kinases. The activity of a multifunctional phosphodiesterase is analysed in chapter 3, using electrospray - tandem mass spectrometric techniques. This includes the differentiation and relative quantification of the isomeric products of the active enzyme preparation and the effect of several cyclic nucleotide binding agents on the enzyme activity. In chapter 4 mass spectrometric data is obtained for two lots of a diagnostic drug, manufactured by two distinct synthetic routes, and for a number of related substances, the aim being to help the manufacturer to optimise the synthetic process. Micro liquid chromatography - atmospheric pressure chemical ionisation - mass spectrometry proved to be the technique of choice for the screening of residues of sulphonamides in milk. In chapter 5, this technique is compared with conventional high performance liquid chromatography with atmospheric pressure chemical ionisation - mass spectrometric detection and capillary zone electrophoresis with electrospray - mass spectrometric detection. The former technique is sensitive and selective allowing the quantification and confirmation of the presence of 10 sulphonamides at levels below the regulatory levels in milk.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available