Multidimensional Liquid Chromatography Theory and Applications in Industrial Chemistry and the Life Sciences
, by Cohen, Steven A.; Schure, Mark R.
- ISBN: 9780471738473 | 0471738476
- Cover: Hardcover
- Copyright: 4/4/2008
Multidimensional Liquid Chromatography (MDLC) is a very powerful separation technique for analyzing exceptionally complex samples in one step. This authoritative reference presents a number of recent contributions that help define the current art and science of MDLC. Topics covered include instrumentation, theory, methods development, and applications of MDLC in the life sciences and in industrial chemistry. With the information to help you perform very difficult separations of complex samples, this reference includes chapters contributed by leading experts or teams of experts.
Steven A. Cohen, PhD, is Life Sciences Director, RDE of the Proteomics Technology Group at the Waters Corporation in Milford, Massachusetts.
MARK R. SCHURE, PhD, is Technical Director of the Computational Chemistry Group and Technical Director of the Theoretical Separation Science Laboratory at the Rohm and Haas Company in Springhouse, Pennsylvania.
| Foreword | p. xiii |
| Preface | p. xv |
| Contributors | p. xvii |
| Introduction | p. 1 |
| Previous Literature Which Covers MDLC | p. 4 |
| How this Book is Organized | p. 5 |
| References | p. 6 |
| Theory | p. 9 |
| Elements of the Theory of Multidimensional Liquid Chromatography | p. 11 |
| Introduction | p. 11 |
| Peak Capacity | p. 13 |
| Resolution | p. 17 |
| Orthogonality | p. 19 |
| Two-Dimensional Theory of Peak Overlap | p. 21 |
| Dimensionality, Peak Ordering, and Clustering | p. 23 |
| Theory of Zone Sampling | p. 24 |
| Dilution and Limit of Detection | p. 26 |
| Chemometric Analysis | p. 27 |
| Future Directions | p. 28 |
| References | p. 30 |
| Peak Capacity in Two-Dimensional Liquid Chromatography | p. 35 |
| Introduction | p. 35 |
| Theory | p. 37 |
| Procedures | p. 41 |
| Results and Discussion | p. 42 |
| Conclusions | p. 49 |
| Generation of Random Correlated Coordinates | p. 50 |
| Derivation of Limiting Correlation Coefficient r | p. 54 |
| References | p. 56 |
| Decoding Complex 2D Separations | p. 59 |
| Introduction | p. 59 |
| Fundamentals: The Statistical Description of Complex Multicomponent Separations | p. 62 |
| Decoding 1D and 2D Multicomponent Separations by Using the SMO Poisson Statistics | p. 68 |
| Decoding Multicomponent Separations by the Autocovariance Function | p. 74 |
| Application to 2D Separations | p. 78 |
| Results from SMO Method | p. 81 |
| Results from 2D Autocovariance Function Method | p. 84 |
| Concluding Remarks | p. 88 |
| Acknowledgments | p. 88 |
| References | p. 88 |
| Columns, Instrumentation and Methods Development | p. 91 |
| Instrumentation for Comprehensive Multidimensional Liquid Chromatography | p. 93 |
| Introduction | p. 93 |
| Heart-Cutting Versus Comprehensive Mode | p. 95 |
| Chromatographic Hardware | p. 97 |
| Valves | p. 97 |
| CE Interfaces | p. 104 |
| Gated Interface for HPLC-CE | p. 104 |
| Microfluidic Valves for On-Chip Multidimensional Analysis | p. 105 |
| Columns and Combinations | p. 106 |
| Column Systems, Dilution, and Splitting | p. 108 |
| Detection | p. 109 |
| Computer Hardware and Software | p. 109 |
| Software Development | p. 110 |
| Valve Sequencing | p. 111 |
| Data Format and Storage | p. 113 |
| Zone Visualization | p. 115 |
| Contour Visualization | p. 115 |
| 2D Peak Presentation | p. 117 |
| Zone Visualization in Specific Chemical (pI) Regions | p. 117 |
| External Plotting Programs | p. 117 |
| Difference Plots | p. 118 |
| Multi-channel Data | p. 118 |
| Data Analysis and Signal Processing | p. 119 |
| Future Prospects | p. 120 |
| References | p. 121 |
| Method Development in Comprehensive Multidimensional Liquid Chromatography | p. 127 |
| Introduction | p. 127 |
| Previous Work | p. 128 |
| Column Variables | p. 130 |
| Method Development | p. 130 |
| The Cardinal Rules of 2DLC Method Development | p. 132 |
| Planning the Experiment | p. 143 |
| General Comments on Optimizing the 2DLC Experiment: Speed-Resolution Trade-off | p. 143 |
| Acknowledgment | p. 144 |
| References | p. 144 |
| Monolithic Columns and Their 2D-HPLC Applications | p. 147 |
| Introduction | p. 147 |
| Monolithic Polymer Columns | p. 148 |
| Structural Properties of Polymer Monoliths | p. 148 |
| Chromatographic Properties of Polymer Monolithic Columns | p. 150 |
| Two-Dimensional HPLC Using Polymer Monoliths | p. 152 |
| Monolithic Silica Columns | p. 153 |
| Preparation | p. 154 |
| Structural Properties of Monolithic Silica Columns | p. 154 |
| Chromatographic Properties of Monolithic Silica Columns | p. 156 |
| Peak Capacity Increase by Using Monolithic Silica Columns in Gradient Elution | p. 158 |
| 2D HPLC Using Monolithic Silica Columns | p. 159 |
| RP-RP 2D HPLC Using Two Different Columns | p. 161 |
| RP-RP 2D HPLC Using Two Similar Columns | p. 164 |
| Ion Exchange-Reversed-Phase 2D HPLC Using a Monolithic Column for the 2nd-D | p. 166 |
| IEX-RP 2D HPLC Using a Monolithic RP Capillary Column for the 2nd-D | p. 168 |
| Summary and Future Improvement of 2D HPLC | p. 171 |
| References | p. 171 |
| Ultrahigh Pressure Multidimensional Liquid Chromatography | p. 177 |
| Background: MDLC in the Jorgenson Lab | p. 177 |
| Cation Exchange-Size Exclusion | p. 178 |
| Anion Exchange-Reversed Phase | p. 180 |
| Cation Exchange-Reversed Phase | p. 181 |
| Size Exclusion-Reversed Phase | p. 183 |
| Online Versus Off-Line MDLC | p. 188 |
| MDLC Using Ultrahigh Pressure Liquid Chromatography: Benefits and Challenges | p. 189 |
| An Introduction to UHPLC | p. 190 |
| UHPLC for LC x LC: High Speed Versus High Peak Capacity | p. 191 |
| LC x UHPLC for Separations of Intact Proteins | p. 191 |
| Experimental Details | p. 193 |
| Instrumentation | p. 193 |
| Data Analysis | p. 194 |
| Chromatographic Conditions | p. 195 |
| Samples | p. 196 |
| Results and Discussion | p. 196 |
| Future Directions for UHP-MDLC | p. 202 |
| References | p. 203 |
| Life Science Applications | p. 205 |
| Peptidomics | p. 207 |
| State of the Art-Why Peptidomics? | p. 207 |
| Strategies and Solutions | p. 208 |
| Summary and Conclusions | p. 218 |
| References | p. 218 |
| A Two-Dimensional Liquid Mass Mapping Technique for Biomarker Discovery | p. 221 |
| Introduction | p. 221 |
| Methods for Separating and Identifying Proteins | p. 223 |
| pI-Based Methods of Separation | p. 223 |
| Chromatofocusing-A Column Based pH Separation | p. 225 |
| Nonporous Separation of Proteins | p. 226 |
| Electrospray-Time of Flight-Mass Spectrometry | p. 228 |
| MALDI Peptide Mass Fingerprinting | p. 229 |
| Data Analysis and Recombination | p. 230 |
| Applications | p. 230 |
| Proteomic Mapping and Clustering of Multiple Samples-Application to Ovarian Cancer Cell Lines | p. 230 |
| 2D Liquid Mass Mapping of Tumor Cell Line Secreted Samples, Application to Metastasis-Associated Protein Profiles | p. 233 |
| Identification Annotation and Data Correlation in MCF10 Human Breast Cancer Cell Lines | p. 235 |
| Summary and Conclusions | p. 237 |
| Acknowledgments | p. 238 |
| References | p. 238 |
| Coupled Multidimensional Chromatography and Tandem Mass Spectrometry Systems for Complex Peptide Mixture Analysis | p. 243 |
| SCX-RP/MS/MS | p. 245 |
| SCX/RP/MS/MS | p. 248 |
| MudPIT | p. 251 |
| Alternative First Dimension Approaches | p. 254 |
| Conclusion | p. 255 |
| References | p. 255 |
| Development of Orthogonal 2DLC Methods for Separation of Peptides | p. 261 |
| Introduction | p. 261 |
| Previous Work | p. 263 |
| Developing Orthogonal 2DLC Methods | p. 264 |
| LC Selectivity for Peptides: Experimental Design | p. 264 |
| Investigation of 2DLC Orthogonality for Separation of Peptides | p. 266 |
| Geometric Approach to Orthogonality in 2DLC | p. 271 |
| Practical 2DLC Considerations in Proteome Research | p. 275 |
| Evaluation of Selected 2DLC MS/MS Systems | p. 276 |
| Peak Capacity in 2DLC-MS/MS | p. 280 |
| Considerations of Concentration Dynamic Range | p. 282 |
| Conclusions | p. 284 |
| Acknowledgment | p. 284 |
| References | p. 284 |
| Multidimensional Separation of Proteins with Online Electrospray Time-of-Flight Mass Spectrometric Detection | p. 291 |
| Introduction | p. 291 |
| Chromatographic Parameters | p. 293 |
| Analyte Detection and Subsequent Analysis | p. 293 |
| Building a Multidimensional Protein Separation | p. 294 |
| Selection of an Ion-Exchange-Reversed-Phase Separation System for Protein-Level Separations | p. 295 |
| Chromatographic Sorbent Considerations | p. 295 |
| Chromatographic Behavior of Proteins | p. 296 |
| Comprehensive Multidimensional Chromatographic Systems | p. 296 |
| Coupling 2DLC with Online ESI-MS Detection | p. 299 |
| Interactions between the Two Dimensions of Chromatography (Step Vs. Linear) | p. 304 |
| Recognizing Increased Selectivity in 2DLC Separations | p. 306 |
| Expanding Multidimensional Separations into a "Middle-Out" Approach to Proteomic Analysis | p. 308 |
| Future Directions in Protein MDLC | p. 311 |
| Protein Chromatography | p. 312 |
| MS Analysis of Proteins | p. 313 |
| Data Interpretation | p. 314 |
| Conclusion | p. 314 |
| References | p. 315 |
| Analysis of Enantiomeric Compounds Using Multidimensional Liquid Chromatography | p. 319 |
| Online Achiral-Chiral LC-LC | p. 320 |
| Applications | p. 323 |
| Analysis of Enantiomers in Plasma and Urine | p. 323 |
| Amino Acids | p. 328 |
| Physiological Fluids or Tissues | p. 328 |
| In Food, Beverages, and Other Products | p. 333 |
| Other Applications | p. 334 |
| Analysis of Enantiomers from Plant and Environmental Sources | p. 334 |
| Miscellaneous Applications | p. 336 |
| Conclusion | p. 338 |
| References | p. 339 |
| Multidimensional Separation Using Capillary Electrophoresis | p. 345 |
| Two-Dimensional Capillary Electrophoresis for the Comprehensive Analysis of Complex Protein Mixtures | p. 347 |
| Introduction | p. 347 |
| Previous Work | p. 348 |
| Miniaturized IEF/SDS-PAGE | p. 348 |
| One-Dimensional Capillary Electrophoresis for Protein Analysis | p. 349 |
| Two-Dimensional Capillary Separations for Analysis of Peptides and Proteins | p. 352 |
| Capillary Liquid Chromatography Coupled with Capillary Electrophoresis for Analysis of Unlabeled Peptides and Proteins | p. 352 |
| Two-Dimensional Capillary Electrophoresis for Analysis of Proteins | p. 352 |
| High-Speed Two-Dimensional Capillary Electrophoresis | p. 356 |
| The Analysis of a Single Fixed Cell | p. 358 |
| Conclusions | p. 360 |
| Abbreviations | p. 360 |
| References | p. 360 |
| Two-Dimensional HPLC-CE Methods for Protein/Peptide Separation | p. 365 |
| Introduction | p. 365 |
| Off-line Versus Online | p. 366 |
| HPLC Fractionation | p. 366 |
| 2D HPLC-CE | p. 367 |
| CE-MS Detection | p. 368 |
| Applications | p. 370 |
| Concluding Remarks | p. 380 |
| Acknowledgment | p. 381 |
| References | p. 381 |
| Industrial Applications | p. 385 |
| Multidimensional Liquid Chromatography in Industrial Applications | p. 387 |
| Introduction | p. 387 |
| Principles of Multidimensional Liquid Chromatography as Applied to Polymer Analysis | p. 390 |
| Experimental | p. 393 |
| Analysis of Alkylene Oxide-Based Polymers | p. 395 |
| Amphiphilic Polyalkylene Oxides | p. 395 |
| Excipients | p. 399 |
| Polyether Polyols | p. 403 |
| Analysis of Condensation Polymers | p. 406 |
| Polyamides | p. 407 |
| Aromatic Polyesters | p. 414 |
| Aliphatic Polyesters | p. 417 |
| References | p. 420 |
| The Analysis of Surfactants by Multidimensional Liquid Chromatography | p. 425 |
| Introduction | p. 425 |
| Analytical Characterization Methods | p. 428 |
| CE and CGE | p. 429 |
| SEC | p. 430 |
| NPLC | p. 431 |
| RPLC | p. 433 |
| Detection Methods | p. 434 |
| 2DLC | p. 434 |
| RPLC Coupled to SEC | p. 435 |
| NPLC Coupled to RPLC | p. 435 |
| Conclusions | p. 442 |
| References | p. 443 |
| Index | p. 447 |
| Table of Contents provided by Ingram. All Rights Reserved. |
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