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Title: Studies of high speed countercurrent chromatography and liquid chromatography-atmospheric pressure ionisation/mass spectrometry in stereoisomeric separations
Author: Whiteside, R. G.
Awarding Body: University of Wales Swansea
Current Institution: Swansea University
Date of Award: 2001
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This thesis describes studies of High Speed Countercurrent Chromatography (HSCCC) and combined Liquid Chromatography-Mass Spectrometry using atmospheric pressure ionisation techniques (LC-API/MA) is stereoisomeric separations related to the pharmaceutical industry. Initially the development of a generic strategy for CCC methodology, which enables this technology to be widely acceptable as a choice for product separation, is discussed. Investigations in the application of HSCCC for chiral separations of diastereomers and enantiomers are also described. Stereoisomeric separations of diastereomers in LC-API/MS are described. In addition, the novel application of enantiomeric separations using cyclodextrin additives in LC-API/MS, are discussed. Chapter 1 gives a general introduction to the thesis. Chapter 2 focuses on the development of a novel generic CCC methodology that can be easily utilised by chromatographers not familiar with CCC technology. Possible correlations between non-chiral separations by CCC, and well established techniques, TLC and HPLC, are discussed through investigations with a range of compounds of varying hydrophobicity using various biphasic solvent systems. The chapter includes an examination of isocratic and gradient elution systems in CCC. Chapter 3 describes the application of cyclodextrins as chiral additives in HPLC and CCC for the enantiomeric separation of chiral drugs. Analytical RP-HPLC is examined as a possible modelling techniques for chiral CCC (Using CDs immobilised in the stationary phase) through investigations of the parameters that effect enantio-separations. This chapter also describes a novel application of the use of on-line mass spectrometry detection for LC chiral separations employing non-volatile cyclodextrins in the mobile phase. The performance of the MS detector is discussed, with regards to reproducibility, linear range of calibration and limits of detection. Optimisation of CCC for the isolation of two pairs of diastereomers from the cinchona alkaloid family; cinchonine and cinchonidine and quinine and quinidine is discussed in chapter 4.
Supervisor: Not available Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available