Contributors ix
Preface xi
1 Introduction 1
Luigi Mondello, Peter Q. Tranchida, and Keith D. Bartle
1.1 Two-Dimensional Chromatography-Mass Spectrometry: A 50-Year-Old Combination, 2
1.2 Shortcomings of One-Dimensional Chromatography, 3
1.3 Benefits of Two-Dimensional Chromatography, 6
1.4 Book Content, 7
1.5 Final Considerations, 11
2 Multidimensional Gas Chromatography: Theoretical Considerations 13
Leonid M. Blumberg
2.1 Symbols, 15
2.2 One-Dimensional GC, 17
2.3 Comprehensive GC × GC, 31
3 Multidimensional Liquid Chromatography: Theoretical Considerations 65
Pavel Jandera
3.1 Two-Dimensional LC Techniques, 66
3.2 Peak Capacity in HPLC: One- and Multidimensional Separations, 69
3.3 Orthogonality in Two-Dimensional LC-LC Systems, 73
3.4 Sample Dimensionality and Structural Correlations, 75
3.5 Separation Selectivity and Selection of Phase Systems in Two-Dimensional LC-LC, 79
3.6 Programmed Elution in Two-Dimensional HPLC, 81
3.7 Fraction Transfer Modulation in Comprehensive LC × LC: Additional Band Broadening, 87
3.8 Future Perspectives, 89
4 History, Evolution, and Optimization Aspects of Comprehensive Two-Dimensional Gas Chromatography 93
Ahmed Mostafa, Tadeusz G´orecki, Peter Q. Tranchida, and Luigi Mondello
4.1 Fundamentals of GC × GC, 94
4.2 Modulation, 96
4.3 GC × GC Data Interpretation, 97
4.4 GC × GC Instrumentation, 100
4.5 Thermal Modulators, 101
4.6 Comprehensive Two-Dimensional GC Method Optimization, 115
4.7 Final Remarks, 140
5 Flow-Modulated Comprehensive Two-Dimensional Gas Chromatography 145
John V. Seeley
5.1 Timing Requirements of GC × GC Modulators, 145
5.2 Criteria for Evaluating Modulators, 150
5.3 Forms of Modulation, 151
5.4 Single-Stage Flow Modulation, 152
5.5 Two-Stage Flow Modulation, 157
5.6 Summary of Flow Modulators, 167
5.7 Brief Comparison to Thermal Modulation, 169
5.8 Concluding Remarks, 169
6 Comprehensive Two-Dimensional Gas Chromatography Combined with Mass Spectrometry 171
Peter Q. Tranchida, Luigi Mondello, Samuel D. H. Poynter, and Robert A. Shellie
6.1 Instrument Requirements for GC × GC-MS, 173
6.2 Data Processing of GC × GC-TOF MS Results, 180
6.3 Method Translation in GC × GC-MS, 181
6.4 GC × MS, 181
6.5 Conventional and Alternative Modulation Techniques for GC × GC-MS, 184
6.6 GC × GC-MS Applications, 187
6.7 Concluding Remarks, 232
7 Detector Technologies and Applications in Comprehensive Two-Dimensional Gas Chromatography 243
Philip J. Marriott
7.1 Detection in GC × GC, 244
7.2 Comments on GC × GC with Mass Spectrometry, 249
7.3 Flame Ionization Detection in GC × GC, 250
7.4 Electron Capture Detection in GC × GC, 254
7.5 Sulfur Chemiluminescence Detection in GC × GC, 260
7.6 Nitrogen Chemiluminescence Detection in GC × GC, 263
7.7 Atomic Emission Detection in GC × GC, 265
7.8 Thermionic Detection in GC × GC, 267
7.9 Flame Photometric Detection in GC × GC, 269
7.10 Case Study of GC × GC with Selective Detection, 272
7.11 Dual Detection with GC × GC, 274
7.12 Conclusions, 275
8 History, Evolution, and Optimization Aspects of Comprehensive Two-Dimensional Liquid Chromatography 281
Isabelle Fran¸cois, Koen Sandra, and Pat Sandra
8.1 Method Development and Instrumentation, 282
8.2 Technical Problems in Comprehensive Liquid Chromatography, 309
8.3 Detection, 314
8.4 Data Representation, 315
8.5 Instrumentation, 316
8.6 Milestones in Comprehensive Liquid Chromatography, 317
8.7 Applications, 320
8.8 Beyond Two-Dimensional Chromatography, 320
8.9 Comparison of LC × LC and Off-Line 2D LC, 321
8.10 Conclusions, 325
9 Comprehensive Two-Dimensional Liquid Chromatography Combined with Mass Spectrometry 331
Paola Dugo, Luigi Mondello, Francesco Cacciola, and Paola Donato
9.1 HPLC-MS, 332
9.2 LC × LC-MS Instrumentation and Method Development, 334
9.3 LC × LC-MS Applications, 336
10 Comprehensive Two-Dimensional Liquid Chromatography Applications 391
Paola Dugo, Luigi Mondello, Francesco Cacciola, and Paola Donato
10.1 Comprehensive 2D LC Separation of Synthetic and Natural Polymers, 392
10.2 Comprehensive 2D LC Separation of Natural Products and Antioxidants, 399
10.3 Comprehensive 2D LC Separation of Pharmaceutical and Environmental Compounds, 412
10.4 Comprehensive 2D LC Separation of Proteins and Peptides, 417
11 Other Comprehensive Chromatography Methods 429
Isabelle Fran¸cois, Pat Sandra, Danilo Sciarrone, and Luigi Mondello
11.1 Online Two-Dimensional Liquid Chromatography-Gas Chromatography, 430
11.2 Online Two-Dimensional Supercritical Fluid Chromatography-Gas Chromatography, 440
11.3 Online Two-Dimensional Supercritical Fluid Chromatography-Supercritical Fluid Chromatography, 440
11.4 Online Two-Dimensional Supercritical Fluid Chromatography-Liquid Chromatography, 442
12 Comprehensive Chromatography Data Interpretation Technologies 449
Elizabeth M. Humston and Robert E. Synovec
12.1 Higher-Order Data Structure, 450
12.2 Modifications of First-Order Data-Handling Approaches, 453
12.3 Visualization, 456
12.4 Mass Spectral Detection, 461
12.5 Chemometrics, 463
12.6 Summary of Data Interpretation Technologies, 472
Index 477
