Multidimensional Liquid Chromatography
Editat de Steven A Cohen, Mark R Schureen Limba Engleză Hardback – mar 2008
Multidimensional Liquid Chromatography (MDLC) is a very powerfulseparation technique for analyzing exceptionally complex samples in onestep. 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 readers perform very difficult separations of complex samples, this reference:
- Includes introductory chapters on theory and instrumentation
- Focuses on techniques that incorporate separations carried out in the liquid phase and by columns, and on those in which the use of the comprehensive mode prevails but is not exclusive
- Covers applications to research in polymer and industrial analysis, pharmaceuticals, and proteomics and other life sciences
- Features chapters contributed by leading experts or teams of experts
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Specificații
ISBN-13: 9780471738473
ISBN-10: 0471738476
Pagini: 480
Dimensiuni: 162 x 244 x 30 mm
Greutate: 0.83 kg
Editura: Wiley
Locul publicării:Hoboken, United States
ISBN-10: 0471738476
Pagini: 480
Dimensiuni: 162 x 244 x 30 mm
Greutate: 0.83 kg
Editura: Wiley
Locul publicării:Hoboken, United States
Public țintă
Analytical chemists in various industries; Pharmaceutical and life science researchers, particularly people who do "–omics" research; Graduate students and post–doctoral fellows in academic laboratories.Notă biografică
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.
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.
Cuprins
Foreword xiii
Preface xv
Contributors xvii
1 Introduction 1
1.1 Previous Literature Which Covers MDLC 4
1.2 How this Book is Organized 5
Part I Theory 9
2 Elements of the Theory of Multidimensional Liquid Chromatography 11
2.1 Introduction 11
2.2 Peak Capacity 13
2.3 Resolution 17
2.4 Orthogonality 19
2.5 Two-Dimensional Theory of Peak Overlap 21
2.6 Dimensionality, Peak Ordering, and Clustering 23
2.7 Theory of Zone Sampling 24
2.8 Dilution and Limit of Detection 26
2.9 Chemometric Analysis 27
2.10 Future Directions 28
3 Peak Capacity in Two-Dimensional Liquid Chromatography 35
3.1 Introduction 35
3.2 Theory 37
3.3 Procedures 41
3.4 Results and Discussion 42
3.5 Conclusions 49
4 Decoding Complex 2D Separations 59
4.1 Introduction 59
4.2 Fundamentals: The Statistical Description of Complex Multicomponent Separations 62
4.3 Decoding 1D and 2D Multicomponent Separations by Using the SMO Poisson Statistics 68
4.4 Decoding Multicomponent Separations by the Autocovariance Function 74
4.5 Application to 2D Separations 78
4.6 Concluding Remarks 88
Part II Columns, Instrumentation and Methods Development 91
5 Instrumentation for Comprehensive Multidimensional Liquid Chromatography 93
5.1 Introduction 93
5.2 Heart-Cutting Versus Comprehensive Mode 95
5.3 Chromatographic Hardware 97
5.4 CE Interfaces 104
5.5 Columns and Combinations 106
5.6 Detection 109
5.7 Computer Hardware and Software 109
5.8 Zone Visualization 115
5.9 Data Analysis and Signal Processing 119
5.10 Future Prospects 120
6 Method Development in Comprehensive Multidimensional Liquid Chromatography 127
6.1 Introduction 127
6.2 Previous Work 128
6.3 Column Variables 130
6.4 Method Development 130
6.5 Planning the Experiment 143
6.6 General Comments on Optimizing the 2DLC Experiment: Speed-Resolution Trade-off 143
7 Monolithic Columns and Their 2D-HPLC Applications 147
7.1 Introduction 147
7.2 Monolithic Polymer Columns 148
7.3 Monolithic Silica Columns 153
7.4 Peak Capacity Increase by Using Monolithic Silica Columns in Gradient Elution 158
7.5 2D HPLC Using Monolithic Silica Columns 159
7.6 Summary and Future Improvement of 2D HPLC 171
8 Ultrahigh Pressure Multidimensional Liquid Chromatography 177
8.1 Background: MDLC in the Jorgenson Lab 177
8.2 Online Versus Off-Line MDLC 188
8.3 MDLC Using Ultrahigh Pressure Liquid Chromatography: Benefits and Challenges 189
8.4 Experimental Details 193
8.5 Results and Discussion 196
8.6 Future Directions for UHP-MDLC 202
Part III Life Science Applications 205
9 Peptidomics 207
9.1 State of the Art-Why Peptidomics? 207
9.2 Strategies and Solutions 208
9.3 Summary and Conclusions 218
10 A Two-Dimensional Liquid Mass Mapping Technique for Biomarker Discovery 221
10.1 Introduction 221
10.2 Methods for Separating and Identifying Proteins 223
10.3 Applications 230
10.4 Summary and Conclusions 237
11 Coupled Multidimensional Chromatography and Tandem Mass Spectrometry Systems for Complex Peptide Mixture Analysis 243
11.1 Scx-rp/ms/ms 245
11.2 Scx/rp/ms/ms 248
11.3 MudPIT 251
11.4 Alternative First Dimension Approaches 254
11.5 Conclusion 255
12 Development of Orthogonal 2DLC Methods for Separation of Peptides 261
12.1 Introduction 261
12.2 Previous Work 263
12.3 Developing Orthogonal 2DLC Methods 264
12.4 Conclusions 284
13 Multidimensional Separation of Proteins with Online Electrospray Time-of-Flight Mass Spectrometric Detection 291
13.1 Introduction 291
13.2 Chromatographic Parameters 293
13.3 Analyte Detection and Subsequent Analysis 293
13.4 Building a Multidimensional Protein Separation 294
13.5 Comprehensive Multidimensional Chromatographic Systems 296
13.6 Coupling 2DLC with Online ESI-MS Detection 299
13.7 Expanding Multidimensional Separations into a 'Middle-Out' Approach to Proteomic Analysis 308
13.8 Future Directions in Protein MDLC 311
13.9 Conclusion 314
14 Analysis of Enantiomeric Compounds Using Multidimensional Liquid Chromatography 319
14.1 Online Achiral-Chiral LC-LC 320
14.2 Applications 323
14.3 Amino Acids 328
14.4 Other Applications 334
14.5 Miscellaneous Applications 336
4.6 Conclusion 338
Part IV Multidimensional Separation Using Capillary Electrophoresis 345
15 Two-Dimensional Capillary Electrophoresis for the Comprehensive Analysis of Complex Protein Mixtures 347
15.1 Introduction 347
15.2 Previous Work 348
15.3 Two-Dimensional Capillary Separations for Analysis of Peptides and Proteins 352
15.4 Conclusions 360
15.5 Abbreviations 360
16 Two-Dimensional HPLC-CE Methods for Protein/Peptide Separation 365
16.1 Introduction 365
16.2 Off-line Versus Online 366
16.3 HPLC Fractionation 366
16.4 2d Hplc-ce 367
16.5 CE-MS Detection 368
16.6 Applications 370
16.7 Concluding Remarks 380
Part V Industrial Applications 385
17 Multidimensional Liquid Chromatography in Industrial Applications 387
17.1 Introduction 387
17.2 Principles of Multidimensional Liquid Chromatography as Applied to Polymer Analysis 390
17.3 Experimental 393
17.4 Analysis of Alkylene Oxide-Based Polymers 395
17.5 Excipients 399
17.6 Polyether Polyols 403
17.7 Analysis of Condensation Polymers 406
17.8 Polyamides 407
17.9 Aromatic Polyesters 414
17.10 Aliphatic Polyesters 417
18 The Analysis of Surfactants by Multidimensional Liquid Chromatography 425
18.1 Introduction 425
18.2 Analytical Characterization Methods 428
18.3 Detection Methods 434
18.4 2dlc 434
18.5 Conclusions 442
References 443
Index 447
Preface xv
Contributors xvii
1 Introduction 1
1.1 Previous Literature Which Covers MDLC 4
1.2 How this Book is Organized 5
Part I Theory 9
2 Elements of the Theory of Multidimensional Liquid Chromatography 11
2.1 Introduction 11
2.2 Peak Capacity 13
2.3 Resolution 17
2.4 Orthogonality 19
2.5 Two-Dimensional Theory of Peak Overlap 21
2.6 Dimensionality, Peak Ordering, and Clustering 23
2.7 Theory of Zone Sampling 24
2.8 Dilution and Limit of Detection 26
2.9 Chemometric Analysis 27
2.10 Future Directions 28
3 Peak Capacity in Two-Dimensional Liquid Chromatography 35
3.1 Introduction 35
3.2 Theory 37
3.3 Procedures 41
3.4 Results and Discussion 42
3.5 Conclusions 49
4 Decoding Complex 2D Separations 59
4.1 Introduction 59
4.2 Fundamentals: The Statistical Description of Complex Multicomponent Separations 62
4.3 Decoding 1D and 2D Multicomponent Separations by Using the SMO Poisson Statistics 68
4.4 Decoding Multicomponent Separations by the Autocovariance Function 74
4.5 Application to 2D Separations 78
4.6 Concluding Remarks 88
Part II Columns, Instrumentation and Methods Development 91
5 Instrumentation for Comprehensive Multidimensional Liquid Chromatography 93
5.1 Introduction 93
5.2 Heart-Cutting Versus Comprehensive Mode 95
5.3 Chromatographic Hardware 97
5.4 CE Interfaces 104
5.5 Columns and Combinations 106
5.6 Detection 109
5.7 Computer Hardware and Software 109
5.8 Zone Visualization 115
5.9 Data Analysis and Signal Processing 119
5.10 Future Prospects 120
6 Method Development in Comprehensive Multidimensional Liquid Chromatography 127
6.1 Introduction 127
6.2 Previous Work 128
6.3 Column Variables 130
6.4 Method Development 130
6.5 Planning the Experiment 143
6.6 General Comments on Optimizing the 2DLC Experiment: Speed-Resolution Trade-off 143
7 Monolithic Columns and Their 2D-HPLC Applications 147
7.1 Introduction 147
7.2 Monolithic Polymer Columns 148
7.3 Monolithic Silica Columns 153
7.4 Peak Capacity Increase by Using Monolithic Silica Columns in Gradient Elution 158
7.5 2D HPLC Using Monolithic Silica Columns 159
7.6 Summary and Future Improvement of 2D HPLC 171
8 Ultrahigh Pressure Multidimensional Liquid Chromatography 177
8.1 Background: MDLC in the Jorgenson Lab 177
8.2 Online Versus Off-Line MDLC 188
8.3 MDLC Using Ultrahigh Pressure Liquid Chromatography: Benefits and Challenges 189
8.4 Experimental Details 193
8.5 Results and Discussion 196
8.6 Future Directions for UHP-MDLC 202
Part III Life Science Applications 205
9 Peptidomics 207
9.1 State of the Art-Why Peptidomics? 207
9.2 Strategies and Solutions 208
9.3 Summary and Conclusions 218
10 A Two-Dimensional Liquid Mass Mapping Technique for Biomarker Discovery 221
10.1 Introduction 221
10.2 Methods for Separating and Identifying Proteins 223
10.3 Applications 230
10.4 Summary and Conclusions 237
11 Coupled Multidimensional Chromatography and Tandem Mass Spectrometry Systems for Complex Peptide Mixture Analysis 243
11.1 Scx-rp/ms/ms 245
11.2 Scx/rp/ms/ms 248
11.3 MudPIT 251
11.4 Alternative First Dimension Approaches 254
11.5 Conclusion 255
12 Development of Orthogonal 2DLC Methods for Separation of Peptides 261
12.1 Introduction 261
12.2 Previous Work 263
12.3 Developing Orthogonal 2DLC Methods 264
12.4 Conclusions 284
13 Multidimensional Separation of Proteins with Online Electrospray Time-of-Flight Mass Spectrometric Detection 291
13.1 Introduction 291
13.2 Chromatographic Parameters 293
13.3 Analyte Detection and Subsequent Analysis 293
13.4 Building a Multidimensional Protein Separation 294
13.5 Comprehensive Multidimensional Chromatographic Systems 296
13.6 Coupling 2DLC with Online ESI-MS Detection 299
13.7 Expanding Multidimensional Separations into a 'Middle-Out' Approach to Proteomic Analysis 308
13.8 Future Directions in Protein MDLC 311
13.9 Conclusion 314
14 Analysis of Enantiomeric Compounds Using Multidimensional Liquid Chromatography 319
14.1 Online Achiral-Chiral LC-LC 320
14.2 Applications 323
14.3 Amino Acids 328
14.4 Other Applications 334
14.5 Miscellaneous Applications 336
4.6 Conclusion 338
Part IV Multidimensional Separation Using Capillary Electrophoresis 345
15 Two-Dimensional Capillary Electrophoresis for the Comprehensive Analysis of Complex Protein Mixtures 347
15.1 Introduction 347
15.2 Previous Work 348
15.3 Two-Dimensional Capillary Separations for Analysis of Peptides and Proteins 352
15.4 Conclusions 360
15.5 Abbreviations 360
16 Two-Dimensional HPLC-CE Methods for Protein/Peptide Separation 365
16.1 Introduction 365
16.2 Off-line Versus Online 366
16.3 HPLC Fractionation 366
16.4 2d Hplc-ce 367
16.5 CE-MS Detection 368
16.6 Applications 370
16.7 Concluding Remarks 380
Part V Industrial Applications 385
17 Multidimensional Liquid Chromatography in Industrial Applications 387
17.1 Introduction 387
17.2 Principles of Multidimensional Liquid Chromatography as Applied to Polymer Analysis 390
17.3 Experimental 393
17.4 Analysis of Alkylene Oxide-Based Polymers 395
17.5 Excipients 399
17.6 Polyether Polyols 403
17.7 Analysis of Condensation Polymers 406
17.8 Polyamides 407
17.9 Aromatic Polyesters 414
17.10 Aliphatic Polyesters 417
18 The Analysis of Surfactants by Multidimensional Liquid Chromatography 425
18.1 Introduction 425
18.2 Analytical Characterization Methods 428
18.3 Detection Methods 434
18.4 2dlc 434
18.5 Conclusions 442
References 443
Index 447
Descriere
This book describes the theory, methodology, and applications of multidimensional liquid phase separations using liquid chromatography and, in some cases, capillary electrophoresis. It addresses the applications of MDLC with an emphasis on recent advances that have increased the practicality of using the technique in today's laboratory.