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Development of an Intelligent Heart-Cut Liquid Chromatography System for Chiral Analysis of Chemical Processes

Development of an Intelligent Heart-Cut Liquid Chromatography System for Chiral Analysis of Chemical Processes

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Title: Development of an Intelligent Heart-Cut Liquid Chromatography System for Chiral Analysis of Chemical Processes
Author: Bizzari, Nour Majid
Abstract: Multi-dimensional HPLC techniques enable researchers to monitor multiple essential and sometimes, critical quality attributes (CQAs) in parallel. A unique three-column, four-dimension liquid chromatography system employing a two-loop heart-cut strategy is reported. The system is capable of re-circulating effluents from each dimension through a single detector and performing heart-cut operations using a programmable ten-port, two-position heart-cut valve. The first dimension of analysis measures peak ratios of products to reagents while the second dimension offers peak purity of the heart-cut material. The third dimension uses a chiral column to measure the enantiomeric excess (ee) of the chiral analyte and the effluent from the third dimension is re-analyzed via a fourth dimension to determine if any loss of chirality has occurred resulting from the analytical method itself. Performance of the setup was evaluated using the synthesis of Warfarin as a model chemical process.
Subject: Organic chemistry
Keywords: HPLC
Multi-dimensional
Heart-cut
Warfarin
Analysis
Quality attributes
Drug development
Process analytical technology
Recycling
Chemical analysis
Chirality
MACOS
Reaction monitoring
Flow chemistry
API
Buchwald Hartwig Amination
Asymmetric Michael Addition
Multidimensional HPLC
Type: Electronic Thesis or Dissertation
Rights: Author owns copyright, except where explicitly noted. Please contact the author directly with licensing requests.
URI: http://hdl.handle.net/10315/34502
Supervisor: Organ, Michael G. ; Pietro, William
Degree: MSc - Master of Science
Program: Chemistry
Exam date: 2017-11-03
Publish on: 2018-05-28

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