Dabo, Azzedine Abdelah (2019) High resolution NMR based approaches for facilitating chromatography method development. PhD thesis, University of Warwick.

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Abstract

Reversed-Phase High Performance Liquid Chromatography (RP-HPLC) is one of the most widely used techniques for provision of analytical measurement information in the pharmaceutical industry from discovery through to development, clinical and manufacturing analytical laboratories. The pharma industry has been for many years attempting to transform the efficiency of method development and increasingly attention has turned to using in silico methodologies. Pfizer have been at the forefront of developing streamlined workflows and more recently, models for retention time prediction so as to reduce the amount of experimental effort in method development. Many of the in-silico strategies used rely on calculated parameters of the molecules under investigation and to some extent the characteristics of the RP-HPLC stationary phases, but no models yet have captured any measures that capture any description of the multiple and complex analyte – stationary phase-mobile phase interactions within any one RPHPLC method condition.

To accomplish this, 1H high resolution magic angle spinning (HR-MAS) nuclear magnetic resonance (NMR) spin-lattice (T1) and spin-spin (T2) relaxation measurements were carried out to probe site-specific molecular motion of a series of aromatic compounds and reversed phase HPLC stationary phases in two different mobile phases. The NMR relaxation measurements provided insight about the nature of the site-specific interaction between the compounds with different stationary phases.

Item Type:	Thesis (PhD)
Subjects:	Q Science > QC Physics Q Science > QD Chemistry Q Science > QP Physiology
Library of Congress Subject Headings (LCSH):	Nuclear magnetic resonance -- Research, High performance liquid chromatography, Spin-lattice relaxation, Aromatic compounds
Official Date:	April 2019
Dates:	Date Event April 2019 UNSPECIFIED
Institution:	University of Warwick
Theses Department:	Department of Chemistry
Thesis Type:	PhD
Publication Status:	Unpublished
Supervisor(s)/Advisor:	Lewandowski, Józef R. ; Brown, Melissa Hannah
Sponsors:	Pfizer Ltd. ; Engineering and Physical Sciences Research Council
Extent:	xxx, 300 leaves : illustrations, charts
Language:	eng

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