InhaltsangabePreface THE BASIC IDEA AND THE DRIVERS Definitions Monoliths as Heterogeneous Catalysts Monoliths in Chromatographic Separations Conclusion and Perspectives PART I: Preparation SYNTHESIS CONCEPTS AND PREPARATION OF SILICA MONOLITHS Introduction Background and Concepts Synthesis of Silica Monoliths Monolithic Columns Prepared in the Laboratory PREPARATION AND PROPERTIES OF VARIOUS TYPES OF MONOLITHIC SILICA STATIONARY PHASES FOR REVERSED-PHASE, HYDROPHILIC INTERACTION, AND ION-EXCHANGE CHROMATOGRAPHY BASED ON POLYMER-COATED MATERIALS Stationary Phases for Reversed-Phase Chromatography Stationary Phases for Hydrophilic-Interaction Chromatography Separations Stationary Phases for Ion-Exchange Separations Advantages of Polymer-Coated Monolithic Silica Columns PART II: Characterization and Modeling CHARACTERIZATION OF THE PORE STRUCTURE OF MONOLITHIC SILICAS Monolithic Silicas General Aspects Describing Porous Materials Characterization Methods of the Pore Structure of Monolithic Silicas Comparison of the Silica Monolith Mesopore-Characterization Data Comparison of the Silica Monolith Flow-Through Pore-Characterization Data MICROSCOPIC CHARACTERIZATIONS Introduction Preparation of Macroporous Silica Monolith Laser Scanning Confocal Microscope Observation Image Processing Fundamental Parameters ThreeDimensional Observation of Deformations in Confined Geometry MODELING CHROMATOGRAPHIC BAND BROADENING IN MONOLITHIC COLUMNS Introduction The General Plate-Height Model User of the General Plate-Height Model to Predict Band Broadening in TSM Structures Conclusion COMPARISON OF THE PERFORMANCE OF PARTICLE-PACKED AND MONOLITHIC COLUMNS IN HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY Introduction Basic Columns Properties Comparison of the Through-Pore Structures and Related Properties Thermodynamic Properties Kinetic Properties and Column Efficiency Conclusions PART III: Applications QUANTITATIVE STRUCTURE-RETENTION RELATIONSHIPS IN STUDIES OF MONOLITHIC MATERIALS Fundamentals of Quantitative Structure-Retention Relationships (QSSR) Quantitative Relationships between Analyte Hydrophobicity and Retention on Monolithic Columns QSSR Based on Structural Descriptors from Calculation Chemistry LSER on Monolithic Columns Concluding Remarks PERFORMANCE OF SILICA MONOLITHS FOR BASIC COMPOUNDS. SILANOL ACTIVITY Introduction Reproducibility of Commercial Monoliths for Analysis of Bases Activity of Monoliths towards Basic Solutes Contribution of Overload to Peak Shapes of Basic Solutes Van Deemter Plots for Commercial Monoliths Performance of Hybrid Capillary Silica Monoliths for Basic Compounds QUALITY CONTROL OF DRUGS Introduction Analysis of Pharmaceutics Natural Products Analysis Analysis Speed and Performance Method Transfer Separation of Complex Mixtures Monolithic Derivatives and Versatile Application Summary and Conclusions MONOLITHIC STATIONARY PHASES FOR FAST ION CHROMATOGRAPHY Fast Ion Chromatography Historical Development of Fast Ion Chromatography 3 Advantages of the Bimodal Porous Structure of the Silica Monolith Matrix Type and Properties of Silica Monolithic Columns Used in IC Modification of Silica Monoliths for IC Separations Operational Parameters Analytical Applications Future Work MONOLITHIC CHIRAL STATIONARY PHASES FOR LIQUID-PHASE ENANTIOSEPARATION TECHNIQUES Introduction Organic Monolithic Materials for the Separation of Enantiomers SilicaBased Monolithic Materials for the Separation of Enantiomers Summary of the Present State-of-the-Art and Problems to be Solved in the Future HIGHSPEED AND HIGHEFFICIENCY SEPARATIONS BY UTILIZING MONOLITHIC SILICA CAPILLARY COLUMNS Introduction Preparation of Monolithic Silica Capillary Columns Properties of Monolithic Silica Capillary Columns Monolithic Silica Capillary Columns for High-Efficiency Separations Monolithic Silica Capillary Columns for High-Speed Separations Future Considerations SILICA

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Klaus K. Unger studied chemistry at the Technical University of Darmstadt, Germany, where he also received his PhD. From 1977 to 2001 he was a professor in chemistry at the Johannes-Gutenberg University, Mainz, Germany, before heading a research group in bioseparations at Merck KGaA, Darmstadt, Germany, for eight years. His research interests are the design and synthesis of porous materials as adsorbents and catalysts, surface functionalization and characterization, the development of liquid phase separation methods, and multidimensional liquid chromatography in proteomics. After studying chemistry at Kyoto University, Japan, Nobuo Tanaka carried out postdocs in the USA at Pennsylvania, Washington and Northeastern Universities, before returning to Kyoto at the Kyoto Institute of Technology (KIT). Since April 2009 he has been working for GL Sciences, Inc., while working part time for KIT as Professor Emeritus. He is the editor of a journal and on the editorial board of several others. Professor Tanaka`s research interests include the development of chromatographic columns and stationary phases, particularly monolithic silica-based materials, as well as the separation of isotopes, isomers and environmental contaminants. Egidijus Machtejevas was born in Lithuania where he studied chemistry and biotechnology at Kaunas University of Technology. After gaining his PhD in analytical chemistry in 2001 he worked as a post-doc with Prof Unger at Mainz University. He joined the R&D Department at Merck KgaA in Darmstadt in 2008, where he is currently a product manager for chromatography. Egidijus Machtejevas has twenty scientific papers and six book chapters to his name, and his major research areas include multidimensional liquid chromatography, proteomics and the development of monolithic stationary phases for chromatography.

Preface THE BASIC IDEA AND THE DRIVERS Definitions Monoliths as Heterogeneous Catalysts Monoliths in Chromatographic Separations Conclusion and Perspectives PART I: Preparation SYNTHESIS CONCEPTS AND PREPARATION OF SILICA MONOLITHS Introduction Background and Concepts Synthesis of Silica Monoliths Monolithic Columns Prepared in the Laboratory PREPARATION AND PROPERTIES OF VARIOUS TYPES OF MONOLITHIC SILICA STATIONARY PHASES FOR REVERSED-PHASE, HYDROPHILIC INTERACTION, AND ION-EXCHANGE CHROMATOGRAPHY BASED ON POLYMER-COATED MATERIALS Stationary Phases for Reversed-Phase Chromatography Stationary Phases for Hydrophilic-Interaction Chromatography Separations Stationary Phases for Ion-Exchange Separations Advantages of Polymer-Coated Monolithic Silica Columns PART II: Characterization and Modeling CHARACTERIZATION OF THE PORE STRUCTURE OF MONOLITHIC SILICAS Monolithic Silicas General Aspects Describing Porous Materials Characterization Methods of the Pore Structure of Monolithic Silicas Comparison of the Silica Monolith Mesopore-Characterization Data Comparison of the Silica Monolith Flow-Through Pore-Characterization Data MICROSCOPIC CHARACTERIZATIONS Introduction Preparation of Macroporous Silica Monolith Laser Scanning Confocal Microscope Observation Image Processing Fundamental Parameters Three-Dimensional Observation of Deformations in Confined Geometry MODELING CHROMATOGRAPHIC BAND BROADENING IN MONOLITHIC COLUMNS Introduction The General Plate-Height Model User of the General Plate-Height Model to Predict Band Broadening in TSM Structures Conclusion COMPARISON OF THE PERFORMANCE OF PARTICLE-PACKED AND MONOLITHIC COLUMNS IN HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY Introduction Basic Columns Properties Comparison of the Through-Pore Structures and Related Properties Thermodynamic Properties Kinetic Properties and Column Efficiency Conclusions PART III: Applications QUANTITATIVE STRUCTURE-RETENTION RELATIONSHIPS IN STUDIES OF MONOLITHIC MATERIALS Fundamentals of Quantitative Structure-Retention Relationships (QSSR) Quantitative Relationships between Analyte Hydrophobicity and Retention on Monolithic Columns QSSR Based on Structural Descriptors from Calculation Chemistry LSER on Monolithic Columns Concluding Remarks PERFORMANCE OF SILICA MONOLITHS FOR BASIC COMPOUNDS. SILANOL ACTIVITY Introduction Reproducibility of Commercial Monoliths for Analysis of Bases Activity of Monoliths towards Basic Solutes Contribution of Overload to Peak Shapes of Basic Solutes Van Deemter Plots for Commercial Monoliths Performance of Hybrid Capillary Silica Monoliths for Basic Compounds QUALITY CONTROL OF DRUGS Introduction Analysis of Pharmaceutics Natural Products Analysis Analysis Speed and Performance Method Transfer Separation of Complex Mixtures Monolithic Derivatives and Versatile Application Summary and Conclusions MONOLITHIC STATIONARY PHASES FOR FAST ION CHROMATOGRAPHY Fast Ion Chromatography Historical Development of Fast Ion Chromatography 3 Advantages of the Bimodal Porous Structure of the Silica Monolith Matrix Type and Properties of Silica Monolithic Columns Used in IC Modification of Silica Monoliths for IC Separations Operational Parameters Analytical Applications Future Work MONOLITHIC CHIRAL STATIONARY PHASES FOR LIQUID-PHASE ENANTIOSEPARATION TECHNIQUES Introduction Organic Monolithic Materials for the Separation of Enantiomers Silica-Based Monolithic Materials for the Separation of Enantiomers Summary of the Present State-of-the-Art and Problems to be Solved in the Future HIGH-SPEED AND HIGH-EFFICIENCY SEPARATIONS BY UTILIZING MONOLITHIC SILICA CAPILLARY COLUMNS Introduction Preparation of Monolithic Silica Capillary Columns Properties of Monolith ...