Handbook of Advanced Chromatography /Mass Spectrometry Techniques

Description

Handbook of Advanced Chromatography /Mass Spectrometry Techniques is a compendium of new and advanced analytical techniques that have been developed in recent years for analysis of all types of molecules in a variety of complex matrices, from foods to fuel to pharmaceuticals and more. Focusing on areas that are becoming widely used or growing rapidly, this is a comprehensive volume that describes both theoretical and practical aspects of advanced methods for analysis. Written by authors who have published the foundational works in the field, the chapters have an emphasis on lipids, but reach a broader audience by including advanced analytical techniques applied to a variety of fields.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques is the ideal reference for those just entering the analytical fields covered, but also for those experienced analysts who want a combination of an overview of the techniques plus specific and pragmatic details not often covered in journal reports. The authors provide, in one source, a synthesis of knowledge that is scattered across a multitude of literature articles. The combination of pragmatic hints and tips with theoretical concepts and demonstrated applications provides both breadth and depth to produce a valuable and enduring reference manual. It is well suited for advanced analytical instrumentation students as well as for analysts seeking additional knowledge or a deeper understanding of familiar techniques.

Includes UHPLC, HILIC, nano-liquid chromatographic separations, two-dimensional LC-MS (LCxLC), multiple parallel MS, 2D-GC (GCxGC) methodologies for lipids analysis, and more
Contains both practical and theoretical knowledge, providing core understanding for implementing modern chromatographic and mass spectrometric techniques
Presents chapters on the most popular and fastest-growing new techniques being implemented in diverse areas of research

Front Cover 2
Handbook of Advanced Chromatography/Mass Spectrometry Techniques 3
Dedication 4
Handbook of Advanced Chromatography/Mass Spectrometry TechniquesEdited byMichal HolčapekUniversity of Pardubice, Pardubice, ... 5
Copyright 6
Contents 7
List of Contributors 15
Preface 17
1 - THEORY AND PRACTICE OF UHPLC AND UHPLC–MS 19
- 1. INTRODUCTION 19
- 2. BRIEF DESCRIPTION OF ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY AND HISTORICAL BACKGROUND 20
  - 2.1 INTEREST IN SMALL PARTICLES IN LIQUID CHROMATOGRAPHY 20
  - 2.2 INTEREST IN VERY HIGH PRESSURES IN LIQUID CHROMATOGRAPHY 23
  - 2.3 PRELIMINARY WORKS OF J.W. JORGENSON AND M.L. LEE IN ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY 25

Front Cover 2
Handbook of Advanced Chromatography/Mass Spectrometry Techniques 3
Dedication 4
Handbook of Advanced Chromatography/Mass Spectrometry TechniquesEdited byMichal HolčapekUniversity of Pardubice, Pardubice, ... 5
Copyright 6
Contents 7
List of Contributors 15
Preface 17
1 - THEORY AND PRACTICE OF UHPLC AND UHPLC–MS 19
- 1. INTRODUCTION 19
- 2. BRIEF DESCRIPTION OF ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY AND HISTORICAL BACKGROUND 20
  - 2.1 INTEREST IN SMALL PARTICLES IN LIQUID CHROMATOGRAPHY 20
  - 2.2 INTEREST IN VERY HIGH PRESSURES IN LIQUID CHROMATOGRAPHY 23
  - 2.3 PRELIMINARY WORKS OF J.W. JORGENSON AND M.L. LEE IN ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY 25
- 3. KINETIC COMPARISON OF ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY WITH OTHER EXISTING TECHNOLOGIES FOR FAST AND HIGH-RESOLUTIO . 26
  - 3.1 BRIEF PRESENTATION OF THE ALTERNATIVE APPROACHES TO ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY 26
  - 3.2 BEST LIQUID CHROMATOGRAPHY APPROACH IN ISOCRATIC MODE—THEORY AND APPLICATIONS 29
  - 3.3 BEST LIQUID CHROMATOGRAPHY APPROACH IN GRADIENT MODE—THEORY AND APPLICATIONS 32
- 4. PROBLEMS RELATED TO ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY 33
  - 4.1 THE NEED TO WORK WITH A DEDICATED INSTRUMENTATION 34
  - 4.2 THE NEED FOR SPECIFIC COLUMNS COMPATIBLE WITH ULTRAHIGH PRESSURES 35
  - 4.3 THE CHANGES IN SOLVENT PROPERTIES WITH PRESSURE 36
- 5. METHOD TRANSFER FROM HIGH-PRESSURE LIQUID CHROMATOGRAPHY TO ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY 38
  - 5.1 THE RULES FOR ISOCRATIC MODE—THEORY AND APPLICATIONS 38
  - 5.2 THE RULES FOR GRADIENT MODE—THEORY AND APPLICATIONS 39
- 6. FIELDS OF APPLICATION FOR ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY AND RELATED ISSUES 41
  - 6.1 ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY/MASS SPECTROMETRY FOR HIGH THROUGHPUT IN BIOANALYSIS 43
  - 6.2 HIGH RESOLUTION DRUG METABOLISM BY ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY USING QUADRUPOLE TIME-OF-FLIG 44
  - 6.3 ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY FOR MULTIRESIDUE SCREENING 45
  - 6.4 ULTRAHIGH-PRESSURE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY IN METABOLOMICS 46
- 7. CONCLUSION/PERSPECTIVES 48
- REFERENCES 49
- FURTHER READING 56
2 - ADVANCES IN HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY 57
- 1. INTRODUCTION 57
- 2. COLUMNS FOR HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY SEPARATIONS 59
  - 2.1 SILICA GEL AND HYBRID INORGANIC SORBENTS 59
  - 2.2 CHEMICALLY BONDED SILICA-BASED STATIONARY PHASES 60
    - 2.2.1 Amino, Amide Amino Acid, and Peptide Bonded Stationary Phases 60
    - 2.2.2 Diol, Polyethylene Glycol, Thioglycerol, Cyclodextrin, and Sugar Bonded Phases 65
    - 2.2.3 Polysuccinimide Bonded Stationary Phases 66
    - 2.2.4 Other Polymer Coated and Bonded Silica Stationary Phases 67
    - 2.2.5 Zwitterionic and Mixed-Mode Silica Stationary Phases 67
  - 2.3 AQUEOUS NORMAL-PHASE CHROMATOGRAPHY ON HYDROSILATED SILICA PHASES 69
  - 2.4 MONOLITHIC COLUMNS FOR HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY SEPARATIONS 70
    - 2.4.1 Silica Gel and Hybrid Monoliths 70
    - 2.4.2 Organic Polymer Hydrophilic Interaction Liquid Chromatography Columns 71
  - 2.5 HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY COLUMN SURVEY 73
- 3. SEPARATION MECHANISM AND EFFECTS OF THE ADSORBED WATER AND MOBILE PHASE 74
  - 3.1 ADSORPTION OF WATER ON POLAR COLUMNS 74
  - 3.2 MOBILE PHASE IN HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY SEPARATIONS 79
  - 3.3 DUAL HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY/REVERSED-PHASE RETENTION MECHANISM 82
  - 3.4 SAMPLE STRUCTURE AND SELECTIVITY IN HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY 85
  - 3.5 TEMPERATURE EFFECTS 86
- 4. HYDROPHILIC INTERACTION LIQUID CHROMATOGRAPHY MODE IN TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY SEPARATION SYSTEMS 87
- 5. SUMMARY AND PERSPECTIVES FOR FURTHER DEVELOPMENT 90
- REFERENCES 91
- FURTHER READING 102
3 - CHIRAL SEPARATIONS. CHIRAL DYNAMIC CHROMATOGRAPHY IN THE STUDY OF STEREOLABILE COMPOUNDS 107
- 1. INTRODUCTION 107
- 2. DYNAMIC CHROMATOGRAPHY: GENERAL PRINCIPLES 108
- 3. MODELS AVAILABLE TO SIMULATE/ANALYZE DYNAMIC CHROMATOGRAMS 110
- 4. CALCULATION OF FREE ENERGY ACTIVATION BARRIERS AND THEIR ENTHALPIC AND ENTROPIC CONTRIBUTIONS 113
- 5. APPLICATION OF DYNAMIC CHROMATOGRAPHY METHODS WITHIN EXTREME OPERATING CONDITIONS 115
- 6. ULTRA-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY 119
- 7. PERTURBING EFFECTS OF STATIONARY PHASES ON ΔG≠ VALUES MEASURED BY DYNAMIC CHROMATOGRAPHY METHODS 125
- REFERENCES 128
- 8. DYNAMIC CHROMATOGRAPHY AS A TOOL TO QUANTIFY CATALYTIC SITES BONDED ON CHROMATOGRAPHIC SUPPORTS 128
- FURTHER READING 132
4 - SILVER-ION LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY 133
- 1. INTRODUCTION 133
- 2. MECHANISM OF SILVER-ION INTERACTION WITH DOUBLE BONDS 133
- 3. PARAMETERS AFFECTING SILVER-ION HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 135
  - 3.1 TYPES OF SILVER-ION SYSTEMS 135
  - 3.2 MOBILE-PHASE COMPOSITION 136
  - 3.3 TEMPERATURE 137
- 5. RETENTION BEHAVIOR 138
  - 5.1 FATTY ACIDS AND THEIR DERIVATIVES 138
  - 5.2 TRIACYLGLYCEROLS 141
- 4. SILVER-ION HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY IN TWO-DIMENSIONAL HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY 138
- 6. REGIOISOMERIC DETERMINATION OF TRIACYLGLYCEROLS 144
  - 6.1 STANDARDS OF REGIOISOMERS 145
  - 6.2 SILVER-ION HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY OF TRIACYLGLYCEROLS REGIOISOMERS 147
  - 6.3 MASS SPECTROMETRIC IDENTIFICATION AND QUANTITATION OF TRIACYLGLYCEROLS REGIOISOMERS 148
- 7. OTHER SILVER-ION HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY APPLICATIONS 151
- 8. CONCLUSIONS AND PERSPECTIVES 152
- ACKNOWLEDGMENTS 152
- REFERENCES 152
5 - POROUS MONOLITHIC LAYERS AND MASS SPECTROMETRY 159
- 1. MASS TRANSPORT IN CHROMATOGRAPHY 159
- 2. ACCELERATION OF SEPARATIONS 160
  - 2.1 NONPOROUS PARTICLES 160
  - 2.2 SMALL POROUS PARTICLES 160
  - 2.3 CORE–SHELL PARTICLES 161
  - 2.4 CONVECTIVE MASS TRANSPORT 161
- 3. HISTORY OF MONOLITHS 162
  - 3.1 EARLY ATTEMPTS 162
  - 3.2 MODERN HISTORY 163
- 4. SPECIFIC FEATURES OF POROUS POLYMER MONOLITHS 165
- 5. SEPARATIONS USING MONOLITHIC COLUMNS AND MASS SPECTROMETRIC DETECTION 166
- 7. SILICA-BASED LAYERS 167
- 6. MONOLITHS IN LAYER FORMAT 167
- 8. ELECTROSPUN POLYMER LAYERS 169
- 9. ORGANIC POLYMER–BASED LAYERS 171
  - 9.1 PREPARATION OF MONOLITHIC LAYERS 172
    - 9.1.1 Monolithic Spots 172
    - 9.1.2 Continuous Monolithic Layers 173
  - 10. MONOLITHIC LAYERS ENHANCING DESORPTION/IONIZATION 176
  - 11. MONOLITHIC LAYERS FOR THIN-LAYER CHROMATOGRAPHY–MASS SPECTROMETRY 179
    - 11.1 THIN-LAYER CHROMATOGRAPHY SEPARATION AND MASS SPECTROMETRIC DETECTION OF BIOMOLECULES 179
    - 11.2 TWO-DIMENSIONAL THIN-LAYER CHROMATOGRAPHY SEPARATION AND MASS SPECTROMETRIC DETECTION OF BIOMOLECULES 184
  - 12. CONCLUDING REMARKS 191
  - REFERENCES 192
  - FURTHER READING 196
- 6 - NEW MATERIALS FOR STATIONARY PHASES IN LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY 197
  - 1. INTRODUCTION 198
  - 2. CORE–SHELL PARTICLES 199
    - 2.1 PRODUCTION OF CORE–SHELL PARTICLES 199
      - 2.1.1 Layer-By-Layer Process 199
      - 2.1.2 Coacervation Process 200
      - 2.1.3 Micelle Templating 201
      - 2.1.4 Other Core–Shell Particles 201
    - 2.2 MORPHOLOGY OF CORE–SHELL PARTICLES 201
    - 2.3 MASS TRANSFER IN FULLY POROUS AND CORE–SHELL PARTICLES 203
      - 2.3.1 Theoretical Background 203
        
        2.3.1.1 Eddy Diffusion 205
        
        2.3.1.2 Longitudinal Diffusion 205
        
        2.3.1.3 Intraparticle Diffusion 207
      - 2.3.2 Experimental Determination of h–ν Curves for Core–Shell and Fully Porous Particles 208
    - 2.4 KINETIC COLUMN PERFORMANCE 214
  - 3. PARTICLE CHEMISTRIES AND PHASE CHEMISTRIES 219
    - 3.1 PARTICLE CHEMISTRIES 222
    - 3.2 PHASE CHEMISTRIES 224
      - 3.2.1 Liquid Chromatography Phases 224
        
        3.2.1.1 Reversed Phase 224
        
        3.2.1.2 Hydrophilic Interaction Liquid Chromatography Phases 226
        
        3.2.1.3 Mixed-Mode Phases 228
        
        3.2.1.3.1 Reversed-Phase/Ionic Exchange Chromatography Mixed-Mode Phases 230
        
        3.2.1.3.2 Hydrophilic Interaction Liquid Chromatography/Ionic Exchange Chromatography Mixed-Mode Phases 232
        
        3.2.2 Phases for Supercritical Fluid Chromatography 233
        
        3.2.2.2 Achiral 235
        
        3.2.2.1 Chiral 235
        
        REFERENCES 236
      - 7 - INTRODUCTION TO TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY—THEORY AND PRACTICE 245
        
        1. TWO-DIMENSIONAL SEPARATIONS: CORE CONCEPTS 245
        
        1.1 VALUE OF A SECOND DIMENSION OF SEPARATION 245
        
        1.2 CONCEPT OF PEAK CAPACITY 246
        
        1.3 INTRODUCTION TO STATISTICAL OVERLAP THEORY FOR CHROMATOGRAPHY 247
        
        3. NOMENCLATURE 249
        
        4. BRIEF HISTORY AND DEVELOPMENTAL MILESTONES 249
        
        2. SCOPE OF THIS CHAPTER 249
        
        5. PRIMARY THEORETICAL GUIDING PRINCIPLES 253
        
        5.1 COMPLEMENTARITY OF RETENTION MECHANISMS 253
        
        5.1.1 Estimation of Separation Space Usage 253
        
        5.1.2 Correction of Peak Capacities for Incomplete Usage of Separation Space 254
        
        5.1.3 Combinations of Modes 255
        
        5.1.4 Separation Modes Should Be Chosen Carefully 257
        
        5.2 THE CONCEPT OF UNDERSAMPLING 258
        
        5.3 DECIDING WHETHER TO DO ONE- OR TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY 261
        
        5.3.1 Comparison of One- and Two-Dimensional Liquid Chromatography in Terms of Peak Capacity 261
        
        5.3.2 Time to Resolve n Compounds 263
        
        6. IMPORTANT PRACTICAL DETAILS ASSOCIATED WITH IMPLEMENTATION 264
        
        6.1 CONCEPTS FOR DIFFERENT MODES OF TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY SEPARATION 265
        
        6.2 IMPORTANT CHARACTERISTICS OF INSTRUMENT COMPONENTS 268
        
        6.2.1 The Sampling Interface 268
        
        6.2.1.1 Effect of Interface Characteristics on Retention Repeatability 268
        
        6.2.1.2 Effect of Interface Characteristics on Second Dimension Column Stability 270
        
        6.2.2 Pumping Systems 273
        
        6.3 OPTIMIZING FOR DETECTION SENSITIVITY 275
        
        7. METHOD DEVELOPMENT 280
        
        7.1 SELECTION OF TWO-DIMENSIONAL SEPARATION MODE 281
        
        7.2 SELECTION OF COMPLEMENTARY SEPARATIONS 283
        
        7.3 SELECTION OF PARTICLE SIZES AND COLUMN DIMENSIONS 284
        
        7.3.1 First Dimension 284
        
        7.3.2 Second Dimension 285
        
        7.4 SELECTION OF OPERATING CONDITIONS 286
        
        8. DETECTION 288
        
        8.3 BACKGROUND CHARACTERISTICS OF SECOND DIMENSION DETECTION 290
        
        8.1 ACQUISITION SPEED 290
        
        8.4 DETECTION SENSITIVITY 290
        
        8.2 EXTRA-COLUMN DISPERSION 290
        
        9. DATA ANALYSIS, SOFTWARE, AND QUANTITATION 291
        
        9.1 DATA STRUCTURES AND HANDLING 291
        
        9.2 DESIRABLE FEATURES OF SOFTWARE SUPPORTING TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY 291
        
        9.2.1 Instrument Control and Acquisition 292
        
        9.2.2 Data Processing—Peak Finding and Integration 293
        
        9.2.3 Advanced Processing—Application of Chemometric Methods 293
        
        9.3 QUANTITATION 293
        
        10. FURTHER READING—SELECTED REVIEW ARTICLES 295
        
        11. FUTURE OUTLOOK 296
        
        ACKNOWLEDGMENTS 296
        
        REFERENCES 296
        
        8 - RECENT ADVANCES IN COMPREHENSIVE TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY FOR THE ANALYSIS OF NATURAL PRODUCTS 305
        
        1. INTRODUCTION 305
        
        2. ADVANCES IN THEORY 306
        
        3. ADVANCES IN PRACTICE 308
        
        4. INSTRUMENTAL SET-UP AND DATA ANALYSIS 309
        
        5. LC×LC OF NATURAL PRODUCTS 310
        
        5.1 LC×LC OF CAROTENOIDS 310
        
        5.2 LC×LC OF TRIACYLGLYCEROLS 311
        
        5.3 LC×LC OF POLYPHENOLIC ANTIOXIDANTS 313
        
        6. FUTURE PERSPECTIVES 315
        
        REFERENCES 317
        
        FURTHER READING 324
        
        9 - NANO-LIQUID CHROMATOGRAPHIC SEPARATIONS 327
        
        1. INTRODUCTION 329
        
        2. MINIATURIZATION IN LIQUID CHROMATOGRAPHY 330
        
        2.1 SOME THEORETICAL CONSIDERATIONS 330
        
        2.1.1 Effect of Column Internal Diameter on Chromatographic Efficiency 330
        
        2.1.2 Chromatographic Dilution 331
        
        2.2 CAPILLARY COLUMNS 331
        
        2.2.1 Packed Capillary Columns 332
        
        2.2.2 Monolithic Capillary Columns 333
        
        2.2.3 Open Tubular Capillary Columns 336
        
        2.3 NANOFLOW GENERATION 337
        
        2.4 INJECTION DEVICES 337
        
        2.5 DETECTION SYSTEMS 338
        
        2.6 IMPROVING SENSITIVITY IN NANO-LIQUID CHROMATOGRAPHY 338
        
        2.7 HYPHENATION OF NANO-LIQUID CHROMATOGRAPHY WITH OTHER TECHNIQUES 339
        
        2.7.1 CLC/Nano-LC–NMR 339
        
        2.7.2 CLC/Nano-LC–Mass Spectrometry 340
        
        3. APPLICATIONS 342
        
        3.1 PROTEIN/PEPTIDE ANALYSIS 342
        
        3.2 ENVIRONMENTAL ANALYSIS 347
        
        3.3 PHARMACEUTICAL ANALYSIS 353
        
        3.4 FOOD ANALYSIS 359
        
        3.5 MISCELLANEOUS 367
        
        4. CONCLUSIONS AND FUTURE TRENDS 370
        
        REFERENCES 371
        
        10 - MULTIPLE PARALLEL MASS SPECTROMETRY FOR LIQUID CHROMATOGRAPHY 383
        
        1. INTRODUCTION 383
        
        1.1 ATMOSPHERIC PRESSURE CHEMICAL IONIZATION MASS SPECTROMETRY 385
        
        1.1.1 Triacylglycerol Regioisomers 385
        
        1.1.2 Triacylglycerol Enantiomers 388
        
        1.2 ELECTROSPRAY IONIZATION MASS SPECTROMETRY 388
        
        1.2.1 Triacylglycerol Regioisomers by Electrospray Ionization Mass Spectrometry 389
        
        1.3 ATMOSPHERIC PRESSURE PHOTOIONIZATION MASS SPECTROMETRY 389
        
        1.4 MULTIPLE MASS SPECTROMETRY APPROACHES 390
        
        1.4.1 Sequential Analyses by Electrospray Ionization, Atmospheric Pressure Chemical Ionization, and Atmospheric Pressure Photoio 391
        
        1.4.3 Simultaneous Parallel Liquid Chromatography Atmospheric Pressure Ionization Mass Spectrometry 392
        
        1.4.2 Multimode Sources 392
        
        2. EXPERIMENTAL 394
        
        2.1 THE WIRELESS COMMUNICATION CONTACT CLOSURE SYSTEM 394
        
        2.2 ATMOSPHERIC PRESSURE CHEMICAL IONIZATION MASS SPECTROMETRY 396
        
        2.3 ATMOSPHERIC PRESSURE PHOTOIONIZATION MASS SPECTROMETRY 396
        
        2.4 ELECTROSPRAY IONIZATION MASS SPECTROMETRY 397
        
        2.5 OTHER DETECTORS AND PUMPS 397
        
        3. RESULTS 399
        
        3.1 QUADRUPLE PARALLEL MASS SPECTROMETRY #1 (LC1/MS4) 399
        
        3.2 QUADRUPLE PARALLEL MASS SPECTROMETRY #2 (LC1/MS4) 399
        
        3.3 LC×LC WITH QUADRUPLE PARALLEL MASS SPECTROMETRY 407
        
        4. CONCLUSION 413
        
        REFERENCES 413
        
        11 - COMPREHENSIVE GAS CHROMATOGRAPHY METHODOLOGIES FOR THE ANALYSIS OF LIPIDS 425
        
        1. INTRODUCTION 425
        
        2. INSTRUMENTATION AND FUNDAMENTAL OPERATIONAL PARAMETERS 425
        
        2.1 MODULATORS 426
        
        2.1.1 Heat-Based Modulators 426
        
        2.1.2 Cryogenic Modulators 427
        
        2.1.3 Flow Modulators 428
        
        2.2 COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY METHOD OPTIMIZATION 429
        
        2.2.1 Modulation Parameters 429
        
        2.2.2 Stationary-Phase Combinations 430
        
        2.2.3 Carrier-Gas Linear Velocities 432
        
        2.3 DETECTORS 433
        
        3. APPLICATIONS 437
        
        3.1 LIPIDS ANALYSIS 437
        
        3.1.1 Fatty Acid Analysis 438
        
        3.1.2 Other Lipid Compounds 448
        
        3.1.3 Volatiles of Oils and Fats 452
        
        4. FINAL REMARKS 455
        
        REFERENCES 455
        
        12 - ULTRA-HIGH PERFORMANCE SUPERCRITICAL FLUID CHROMATOGRAPHY–MASS SPECTROMETRY 463
        
        1. INTRODUCTION 463
        
        1.1 SUPERCRITICAL FLUIDS 464
        
        1.2 HISTORY OF SUPERCRITICAL FLUID CHROMATOGRAPHY 467
        
        1.3 SEPARATION EFFICIENCY IN SUPERCRITICAL FLUID CHROMATOGRAPHY AND ULTRA-HIGH PERFORMANCE SUPERCRITICAL FLUID CHROMATOGRAPHY 469
        
        2. SUPERCRITICAL FLUID CHROMATOGRAPHY AND ULTRA-HIGH PERFORMANCE SUPERCRITICAL FLUID CHROMATOGRAPHY INSTRUMENTATION 471
        
        2.1 GENERAL FEATURES OF SUPERCRITICAL FLUID CHROMATOGRAPHY INSTRUMENTATION 472
        
        2.1.1 Supercritical Fluid Chromatography Pumps 472
        
        2.1.2 Autosamplers in Supercritical Fluid Chromatography 473
        
        2.1.5 UV Detection 473
        
        2.1.3 Column Oven 473
        
        2.1.4 Backpressure Regulator 473
        
        2.1.6 Evaporative Light Scattering Detector and Charged Aerosol Detector 474
        
        2.2 ULTRA-HIGH PERFORMANCE SUPERCRITICAL FLUID CHROMATOGRAPHY INSTRUMENTATION 475
        
        3. OPERATING PARAMETERS IN SUPERCRITICAL FLUID CHROMATOGRAPHY 476
        
        3.1 MOBILE PHASE 476
        
        3.2 STATIONARY PHASE 480
        
        3.3 BACKPRESSURE AND TEMPERATURE 481
        
        3.4 FLOW-RATE 483
        
        3.5 INJECTION SOLVENT 484
        
        4. INTERFACING SUPERCRITICAL FLUID CHROMATOGRAPHY AND MASS SPECTROMETRY 485
        
        4.1 ION SOURCES AND INTERFACES IN SUPERCRITICAL FLUID CHROMATOGRAPHY–MASS SPECTROMETRY 485
        
        4.2 INTERFACING ATMOSPHERIC PRESSURE IONIZATION TECHNIQUES WITH SUPERCRITICAL FLUID CHROMATOGRAPHY 487
        
        4.3 SUPERCRITICAL FLUID CHROMATOGRAPHY–MASS SPECTROMETRY CONDITIONS 490
        
        5. APPLICATIONS OF SUPERCRITICAL FLUID CHROMATOGRAPHY 491
        
        5.1 PREDOMINANT SUPERCRITICAL FLUID CHROMATOGRAPHY APPLICATIONS 492
        
        5.2 APPLICATIONS OF SUPERCRITICAL FLUID CHROMATOGRAPHY–MASS SPECTROMETRY 493
        
        6. CONCLUSIONS 496
        
        REFERENCES 497
        
        Index 507
        
        A 507
        
        B 507
        
        C 508

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