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Title: Studies of chromatographic and spectroscopic methods for the analysis of anabolic steroids and other drugs
Author: Fowlis, I. A.
Awarding Body: University College of Swansea
Current Institution: Swansea University
Date of Award: 1991
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The objectives of these studies were to develop multidimensional chromatographic techniques and combine them, in some cases with mass spectrometry, in order to provide improved methods for the determination of an anabolic steroid in plasma extracts and for the identification of by-products in drug process waste streams and bulk products. Combination of high pressure liquid chromatography (HPLC) with high resolution capillary gas chromatography (HRGG) was studied using an autosampler as an interface device. Detailed investigations were carried out using liquid chromatography solute preconcentration and optimal conditions for injections of large volumes (1 ml) of polar solutions of solutes in both normal and reverse phase HPLC were established. This resulted in enhanced detection limits whilst maintaining chromatographic resolution with reduction in interferences from endogenous materials. The system was extended by direct interfacing of the HPLC-HRGC to a mass selective mass spectrometer to provide HPLC-HRGC-MS. The normal and reverse phase HPLC preconcentration methods were also inferfaced to a supercritical fluid chromatograph and the HPLC-SFC system was used with ultraviolet and mass spectrometric detection. In addition, a simple headspace focussing procedure was developed and combined with HRGC-MS. The systems developed were used to investigate the analysis of stanozolol in plasma extracts. HPLC-HRGC gave useful results, but problems were encountered due to adsorptive properties of the drug. Studies with HPLC-SFC-MS gave good data which indicated that this form of analysis is worthy of further assessment. Use of HPLC-HRGC-MS, SFC-MS and HPLC-SFC-MS extended the positive identification of by-products in the paracetamol manufacturing process. In particular only these combined methods have enabled benzenediazonium innersalts to be identified. These positive identifications have considerably enhanced understanding of the mass balance study of the chemical process.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available