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Analytical Separations Using Packed and Open-Tubular Capillary Electrochromatography" (2004)

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Analytical Separations Using Packed and Open-Tubular Capillary Electrochromatography Louisiana State University LSU Digital Commons LSU Doctoral Dissertations Graduate School 2004 Analytical separations using packed and open- tubular capillary electrochromatography Constantina P. Kapnissi Louisiana State University and Agricultural and Mechanical College, [email protected] Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_dissertations Part of the Chemistry Commons Recommended Citation Kapnissi, Constantina P., "Analytical separations using packed and open-tubular capillary electrochromatography" (2004). LSU Doctoral Dissertations. 595. https://digitalcommons.lsu.edu/gradschool_dissertations/595 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Doctoral Dissertations by an authorized graduate school editor of LSU Digital Commons. For more information, please [email protected]. ANALYTICAL SEPARATIONS USING PACKED AND OPEN- TUBULAR CAPILLARY ELECTROCHROMATOGRAPHY A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemistry by Constantina P. Kapnissi B.S., University of Cyprus, 1999 August 2004 Copyright 2004 Constantina Panayioti Kapnissi All rights reserved ii DEDICATION I would like to dedicate this work to my husband Andreas Christodoulou, my parents Panayiotis and Eleni Kapnissi, and my sisters Erasmia, Panayiota and Stella Kapnissi. I want to thank all of you for helping me, in your own way, to finally make one of my dreams come true. Thank you for encouraging me to continue and achieve my goals. Thank you for your endless love, support, and motivation. Andreas, thank you for your continuous patience and for being there for me whenever I needed you during this difficult time. I will never forget what you did for me. iii ACKNOWLEDGMENTS I would like to acknowledge the following people for their contributions in this work: Dr. Isiah M. Warner for his guidance and excellent advice. Thank you for encouraging me to finish what I started. I want to also thank you for the financial and moral support. You are an excellent mentor, and you prove that every day with your constant encouragement and support. Thank you again for everything. Dr. Rezik A. Agbaria for his helpful scientific discussions during my general exam and my project with laser scanning confocal microscopy. Dr. Charles William Henry III for training me how to use the capillary electrophoresis instrument and the packing apparatus. Dr. Henry and Dr. Shahab Shamsi helped me understand the most important concepts of my research. Dr. Joseph B. Schlenoff and his group at Florida State University in Tallahassee, Florida for training me on the polyelectrolyte multilayer coating procedure. Dr. Lei Geng and Mark Lowry at University of Iowa in Iowa City, Iowa for helping me conduct some experiments on the laser scanning confocal microscope, and for their helpful discussions about this part of my research. Dr. Akbay Cevdet and Bertha C. Valle for providing the polymeric surfactants I used in my research work. Warner research group and Warner family for their encouragement and their total support. Bertha C. Valle for her friendship, her advice, and the long useful discussions we had about research. iv Dr. Nikki Gill, Dr. Xiaofeng Zhu, and Dr. Abdul Numan for editing a few of my reports. My family and friends in Cyprus for believing in me, and supporting all my choices. v TABLE OF CONTENTS DEDICATION .....................................................................................................................iii ACKNOWLEDGMENTS ...................................................................................................iv LIST OF TABLES ...............................................................................................................ix LIST OF FIGURES ..............................................................................................................x LIST OF ABBREVIATIONS ............................................................................................xiv ABSTRACT .................................................................................................................... xviii CHAPTER 1. INTRODUCTION .........................................................................................1 1.1 Capillary Electrophoresis ....................................................................................1 1.2 Micellar Electrokinetic Chromatography ...........................................................9 1.3 Capillary Electrochromatography .....................................................................15 1.3.1 Packed-Capillary Electrochromatography ...............................................17 1.3.2 Open-Tubular Capillary Electrochromatography ....................................18 1.3.2.1 Adsorption ...................................................................................20 1.3.2.2 Covalent Bonding and/or Crosslinking .......................................29 1.3.2.3 Porous Layers ..............................................................................31 1.3.2.4 Chemical Bonding After Etching ................................................32 1.3.2.5 Sol-Gel Technique .......................................................................35 1.4 Chirality ............................................................................................................38 1.5 Chiral Selectors in Open-Tubular Capillary Electrochromatography ..............40 1.5.1 Derivatized Cyclodextrins .......................................................................40 1.5.2 Cellulose ..................................................................................................42 1.5.3 Proteins ....................................................................................................43 1.5.4 Molecular Imprinted Polymers ................................................................44 1.5.5 Polymeric Surfactants ..............................................................................46 1.6 Laser Scanning Confocal Microscopy ..............................................................47 1.7 Scope of Dissertation ........................................................................................51 1.8 References .........................................................................................................54 CHAPTER 2. SEPARATION OF BENZODIAZEPINES BY USE OF CAPILLARY ELECTROCHROMATOGRAPHY .....................................65 2.1 Introduction .......................................................................................................65 2.2 Experimental .....................................................................................................68 2.2.1 Reagents and Chemicals ..........................................................................68 2.2.2 Instrumentation and Conditions ...............................................................68 2.2.3 Sample and Buffer Preparation ................................................................69 2.2.4 Preparation and Conditioning of Packed Capillary Columns ..................69 2.3 Results and Discussion .....................................................................................70 vi 2.3.1 Effect of the Nature of Organic Modifier ................................................70 2.3.2 Effect of Mobile-Phase Composition ......................................................73 2.3.3 Effect of Applied Voltage ........................................................................73 2.3.4 Effect of Tris Concentration ....................................................................75 2.3.5 Effect of Column Temperature ................................................................76 2.3.6 CEC Separation of Drugs from a Urine Sample ......................................78 2.4 Conclusion ........................................................................................................81 2.5 References .........................................................................................................81 CHAPTER 3. ANALYTICAL SEPARATIONS USING MOLECULAR MICELLES IN OPEN-TUBULAR CAPILLARY ELECTROCHROMATOGRAPHY .....................................85 3.1 Introduction .......................................................................................................85 3.2 Experimental .....................................................................................................87 3.2.1 Apparatus and Conditions ........................................................................87 3.2.2 Reagents and Chemicals ..........................................................................87 3.2.3 Sample and Buffer Preparation ................................................................88 3.2.4 Synthesis of Monomeric and Polymeric Surfactant ................................88 3.2.5 Procedure for Polyelectrolyte Multilayer (PEM) Coating .......................88 3.3 Results and Discussion .....................................................................................89 3.3.1 Endurance of PEM Coating .....................................................................89 3.3.2 Stability of PEM Coating .........................................................................91 3.3.3 Reproducibilities ......................................................................................92
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