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Monolithic Silicas in Separation Science. Concepts, Syntheses, Characterization, Modeling and Applications

  • ID: 2183300
  • Book
  • January 2011
  • 362 Pages
  • John Wiley and Sons Ltd
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Edited by the experts and pioneers in the field, this is the first monograph to cover the topic, containing the must–have information hitherto only scattered among journals.

Clearly divided into sections on preparation, characterization, modeling and applications, this is essential reading for chemists, chromatographers, analytical chemists, biochemists and biologists.
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List of Contributors.

1 The Basic Idea and the Drivers (Nobuo Tanaka and Klaus K. Unger).

1.1 Definitions.

1.2 Monoliths as Heterogeneous Catalysts.

1.3 Monoliths in Chromatographic Separations.

1.4 Conclusion and Perspectives.


Part One Preparation.

2 Synthesis Concepts and Preparation of Silica Monoliths (Kazuki Nakanishi).

2.1 Introduction.

2.2 Background and Concepts.

2.3 Synthesis of Silica Monoliths.

2.4 Monolithic Columns Prepared in the Laboratory.

2.5 Summary.


3 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 (Oscar Nunez and Tohru Ikegami).

3.1 Stationary Phases for Reversed–Phase Chromatography.

3.2 Stationary Phases for Hydrophilic–Interaction Chromatography Separations.

3.3 Stationary Phases for Ion–Exchange Separations.

3.4 Advantages of Polymer–Coated Monolithic Silica Columns.


Part Two Characterization and Modeling.

4 Characterization of the Pore Structure of Monolithic Silicas (Romas Skudas, Matthias Thommes, and Klaus K. Unger).

4.1 Monolithic Silicas.

4.2 General Aspects Describing Porous Materials.

4.3 Characterization Methods of the Pore Structure of Monolithic Silicas.

4.4 Comparison of the Silica Monolith Mesopore–Characterization Data.

4.5 Comparison of the Silica Monolith Flow–Through Pore–Characterization Data.


5 Microscopic Characterizations (Haruko Saito, Kazuyoshi Kanamori, and Kazuki Nakanishi).

5.1 Introduction.

5.2 Preparation of Macroporous Silica Monolith.

5.3 Laser Scanning Confocal Microscope Observation.

5.4 Image Processing.

5.5 Fundamental Parameters.

5.6 Three–Dimensional Observation of Deformations in Confined Geometry.


6 Modeling Chromatographic Band Broadening in Monolithic Columns (Frederik Detobel and Gert Desmet).

6.1 Introduction.

6.2 The General Plate–Height Model.

6.3 Use of the General Plate–Height Model to Predict Band Broadening in TSM Structures.

6.4 Conclusion.



Greek Symbols.



7 Comparison of the Performance of Particle–Packed and Monolithic Columns in High–Performance Liquid Chromatography (Georges Guiochon).

7.1 Introduction.

7.2 Basic Columns Properties.

7.3 Comparison of the Through–Pore Structures and Related Properties.

7.4 Thermodynamic Properties.

7.5 Kinetic Properties and Column Efficiency.

7.6 Conclusions.



Greek Symbols.


Part Three Applications.

8 Quantitative Structure Retention Relationships in Studies of Monolithic Materials (Roman Kaliszan and Micha J. Markuszewski).

8.1 Fundamentals of Quantitative Structure Retention Relationships (QSRR).

8.2 Quantitative Relationships between Analyte Hydrophobicity and Retention on Monolithic Columns.

8.3 QSRR Based on Structural Descriptors from Calculation Chemistry.

8.4 LSER on Monolithic Columns.

8.5 Concluding Remarks.


9 Performance of Silica Monoliths for Basic Compounds. Silanol Activity (David V. McCalley).

9.1 Introduction.

9.2 Reproducibility of Commercial Monoliths for Analysis of Bases.

9.3 Activity of Monoliths towards Basic Solutes.

9.4 Contribution of Overload to Peak Shapes of Basic Solutes.

9.5 Van Deemter Plots for Commercial Monoliths.

9.6 Performance of Hybrid Capillary Silica Monoliths for Basic Compounds.

9.7 Conclusions.


10 Quality Control of Drugs (Mohammed Taha, Abdelkarem Abed, and Sami El Deeb).

10.1 Introduction.

10.2 Analysis of Pharmaceutics.

10.3 Natural Products Analysis.

10.4 Analysis Speed and Performance.

10.5 Method Transfer.

10.6 Separation of Complex Mixtures.

10.7 Monolith Derivatives and Versatile Application.

10.8 Summary and Conclusions.


11 Monolithic Stationary Phases for Fast Ion Chromatography (Pavel N. Nesterenko and Paul R. Haddad).

11.1 Fast Ion Chromatography.

11.2 Historical Development of Fast Ion Chromatography.

11.4 Type and Properties of Silica Monolithic Columns Used in IC 212.

11.5 Modification of Silica Monoliths for IC Separations.

11.6 Operational Parameters.

11.7 Analytical Applications.

11.8 Future Work.


12 Monolithic Chiral Stationary Phases for Liquid–Phase Enantioseparation Techniques (Bezhan Chankvetadze).

12.1 Introduction.

12.2 Organic Monolithic Materials for the Separation of Enantiomers.

12.3 Silica–Based Monolithic Materials for the Separation of Enantiomers.

12.4 Summary of the Present State–of–the–Art and Problems to be Solved in the Future.


13 High–Speed and High–Effi ciency Separations by Utilizing Monolithic Silica Capillary Columns (Takeshi Hara, Kosuke Miyamoto, Satoshi Makino, Shohei Miwa, Tohru Ikegami, Masayoshi Ohira, and Nobuo Tanaka).

13.1 Introduction.

13.2 Preparation of Monolithic Silica Capillary Columns.

13.3 Properties of Monolithic Silica Capillary Columns.

13.4 Monolithic Silica Capillary Columns for High–Efficiency Separations.

13.5 Monolithic Silica Capillary Columns for High–Speed Separations.

13.6 Future Considerations.

13.7 Conclusion.


14 Silica Monolithic Columns and Mass Spectrometry (Keith Ashman).

14.1 Introduction.

14.2 Offline Chromatography, LC MALDI MS.

14.3 Online ESI LC/MS/MS for Proteomics and Selected Reaction Monitoring (SRM).

14.4 Online Reactors and Affinity Columns Coupled to Mass Spectrometry.

14.5 Conclusion.


15 Silica Monoliths for Small–Scale Purification of Drug–Discovery Compounds (Alfonso Espada, Cristina Anta, and Manuel Molina–Martin).

15.1 Introduction.

15.2 Instrumental and Operating Considerations.

15.3 Preparative Separations and Sample Loading.

15.4 Purification of Drug–Discovery Compounds.

15.5 Conclusions.



16 Monolithic Silica Columns in Multidimensional LC–MS for Proteomics and Peptidomics (Egidijus Machtejevas and Egl Machtejevien ).

16.1 Introduction.

16.2 Liquid Chromatography as a Tool Box for Proteomics.

16.3 Selectivity of Columns for MD–LC.

16.4 Dimensions of Columns in MD–LC.

16.5 Monolithic Silica Columns.

16.6 Applications of Monolithic Silica in Proteomics A Brief Survey.

16.7 Summary and Conclusions.


17 Silica Monoliths in Solid–Phase Extraction and Solid–Phase Microextraction (Zhi–Guo Shi, Li Xu, and Hian Kee Lee).

17.1 Introduction.

17.2 Extraction Process.

17.3 Extraction Platforms.

17.4 Applications.

17.4.1 SPE and SPME. Silica Monolith from Entrapped Particles. Silica Monolith from Direct Sol–Gel Strategy.

17.4.2 Other Applications of Silica Monolith.

17.5 Conclusion and Outlook.



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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.

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