Comprehensive Chromatography in Combination with Mass Spectrometry
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This book provides a detailed description of various multidimensional chromatographic separation techniques. The editor first provides an introduction to the area and then dives right into the various complex separation techniques. While still not used routinely comprehensive chromatography techniques will help acquaint the readers with the fundamentals and possible benefits of multi-dimensional separations coupled with mass spectrometry.

The topics include a wide range of material that will appease all interested in either entering the field of multidimensional chromatography and those looking to gain a better understanding of the topic.


Luigi Mondello is an expert in the field of multidimensional chromatography. He has published a number of books and papers in his field and has been an invited speaker at a number of conferences. He is Editor of the Journal of Separation Science (Wiley). Recently he was awarded The Chromatographic Society's Silver Jubilee Medal award for his work in the field of chromatography and the COLACRO Medal for his contribution to the development and diffusion of the Chromatographic Techniques, and the HTC-Award for the most outstanding and innovative work in the field of hyphenated chromatographic techniques from the Flemish Chemical Society. He is currently Full Professor of Analytical Chemistry at the the University of Messina in Italy and permanent member of the scientific committee of the International Symposium on Capillary Chromatography (ISCC); the International Symposium on Essential Oils (ISEO); the International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers (HTC-11); the Brazilian Symposium on Chromatography and Related Techniques (SIMCRO); and the Congresso Latino-Americano de Cromatografia e Técnicas Relacionades (COLACRO).


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


“It offers comprehensive coverage of the topic of comprehensive multidimensional separations, at a level that makes it a useful reference for scientists working in the field, or as a primary textbook for a graduate-level course on advanced separation techniques.”  (Anal Bioanal Chem, 2012)