Front Cover 1
INSTRUMENTAL THIN-LAYER CHROMATOGRAPHY 4
Copyright 5
Contents 6
Contributors 8
Chapter 1 - Milestones, Core Concepts, and Contrasts 12
1.1 INTRODUCTION 12
1.2 MILESTONES 13
1.3 ATTRIBUTES OF A PLANAR FORMAT 15
1.4 CONSEQUENCES OF CAPILLARY-CONTROLLED FLOW 18
1.5 SOLVENT-STRENGTH GRADIENTS 30
1.6 MULTIDIMENSIONAL SEPARATIONS 33
1.7 CONCLUSIONS 36
References 37
Chapter 2 - High-Performance Precoated Stationary Phases 42
2.1 INTRODUCTION 42
2.2 INORGANIC OXIDE SORBENTS 43
2.3 CHEMICALLY BONDED SORBENTS 50
2.4 CELLULOSE 56
2.5 CHIRAL SORBENTS 57
2.6 CONCLUSIONS 59
References 60
Chapter 3 - Ultrathin and Nanostructured Stationary Phases 64
3.1 INTRODUCTION 64
3.2 MONOLITHIC SILICA GELS 67
3.3 MONOLITHIC POLYMERS 69
3.4 ELECTROSPUN NANOFIBERS 70
3.5 NANOSTRUCTURED THIN FILMS 72
3.6 CARBON NANOTUBE-TEMPLATED LAYERS 75
3.7 ADVANCED INSTRUMENTATION AND TECHNIQUES 77
3.8 CONCLUSIONS 79
References 80
Chapter 4 - Automated Multiple Development 84
4.1 INTRODUCTION 84
4.2 APPLICATIONS 94
4.3 FUTURE TRENDS 105
4.4 CONCLUSIONS 108
References 109
Chapter 5 - Forced-Flow Development in Overpressured Layer Chromatography 118
5.1 INTRODUCTION 118
5.2 ANALYTICAL AND PREPARATIVE OPLC PROCESSES 119
5.3 INSTRUMENTS AND LAYERS FOR OPLC 123
5.4 MAIN CHARACTERISTICS OF OPLC 127
5.5 ANALYTICAL AND PREPARATIVE APPLICATIONS 133
5.6 CONCLUSION 140
References 140
Chapter 6 - Pressurized Planar Electrochromatography 146
6.1 INTRODUCTION 146
6.2 THEORETICAL BACKGROUND 147
6.3 DEVELOPMENT OF EQUIPMENT FOR PPEC 151
6.4 ADVANTAGES OF PPEC 159
6.5 APPLICATIONS 168
6.6 CHALLENGES AND CONCLUSIONS 174
References 174
Chapter 7 - Theory and Instrumentation for In situ Detection 178
7.1 INTRODUCTION 178
7.2 THEORY FOR IN SITU DENSITOMETRIC DETECTION 179
7.3 INSTRUMENTATION FOR IN SITU DENSITOMETRIC DETECTION 187
7.4 IN SITU MASS-SPECTROMETRY 197
7.5 IN SITU RADIOISOTOPE DETECTION 198
References 199
Chapter 8 - Staining and Derivatization Techniques for Visualization in Planar Chromatography 202
8.1 PROBLEM OVERVIEW 202
8.2 REAGENT APPLICATION, EQUIPMENT, AND PROTOCOLS 204
8.3 TECHNIQUES FOR HEATING OR DRYING LAYERS AFTER DEVELOPMENT 212
8.4 COMMON DETECTION PROTOCOLS FOR TARGET COMPOUNDS 215
8.5 CONCLUSIONS 246
References 246
Chapter 9 - Advanced Spectroscopic Detectors for Identification and Quantification: UV–Visible, Fluorescence, and Infrared ... 250
9.1 INTRODUCTION 250
9.2 ADVANCED SPECTROSCOPIC DETECTORS FOR IDENTIFICATION AND QUANTIFICATION 251
9.3 CONCLUSION 258
References 258
Chapter 10 - Advanced Spectroscopic Detectors for Identification and Quantification: Mass Spectrometry 260
10.1 INTRODUCTION 260
10.2 CLASSIFICATION OF TLC-MS TECHNIQUES 261
10.3 INDIRECT SAMPLING TLC-MS 261
10.4 DIRECT SAMPLING TLC-MS 265
10.5 HIGH-THROUGHPUT TLC-MS DEVICES AND QUANTIFICATION ANALYSIS 279
10.6 CONCLUSION 281
References 282
Chapter 11 - Effects-Directed Biological Detection: Bioautography 290
11.1 INTRODUCTION 290
11.2 APPLICATIONS OF BIOAUTOGRAPHIC TESTS 295
11.3 PERSPECTIVES 314
References 314
Chapter 12 - Solvent Selection and Method Development 324
12.1 INTRODUCTION 324
12.2 PROBLEM DEFINITION 325
12.3 MODE SELECTION 330
12.4 MOBILE PHASE SELECTION 334
12.5 CONCLUSIONS 359
References 359
Chapter 13 - Validation of Thin Layer Chromatographic Methods 362
13.1 INTRODUCTION 362
13.2 METHOD VALIDATION USING THE CLASSIC APPROACH 363
13.3 ALTERNATIVE METHOD VALIDATION APPROACH USING ACCURACY PROFILES 372
13.4 CONCLUSION 382
References 382
Chapter 14 - Separation of (Phospho)Lipids by Thin-Layer Chromatography 386
14.1 INTRODUCTION 386
14.2 SEPARATION OF LIPIDS BY TLC 389
14.3 APPLICATIONS 393
14.4 MALDI FOR MS DETECTION 406
14.5 SUMMARY AND OUTLOOK 410
Acknowledgments 410
References 411
Chapter 15 - Applications in Food Analysis 418
15.1 INTRODUCTION 418
15.2 HPTLC IN FOOD ANALYSIS 420
15.3 SAMPLE PREPARATION, HYPHENATION, AND NEW POSSIBILITIES 424
15.4 SUITABILITY AND CAPABILITIES 432
15.5 CONCLUSION 435
References 435
Chapter 16 - Environmental Applications 442
16.1 INTRODUCTION 442
16.2 HPTLC IN ENVIRONMENTAL ANALYSIS 443
16.3 CONCLUSION 455
References 456
Chapter 17 - Pharmaceutical Applications of High Performance Thin Layer Chromatography 462
17.1 INTRODUCTION 462
17.2 QUANTITATIVE ANALYSIS 464
17.3 PHARMACEUTICAL APPLICATIONS 464
17.4 CONCLUSIONS 488
References 488
Chapter 18 - Utility of Thin-Layer Chromatography in the Assessment of the Quality of Botanicals 490
18.1 INTRODUCTION 490
18.2 METHOD VALIDATION 494
18.3 HYPHENATED TECHNIQUES AND CHEMOMETRICS IN HERBAL ANALYSIS 497
18.4 APPLICATIONS OF TLC IN THE FIELD OF HERBAL PRODUCTS/BOTANICALS 499
18.5 USE OF HPTLC BY THE AMERICAN HERBAL PHARMACOPOEIA 511
18.6 RECENT ADVANCES IN HPTLC-BASED QUALITY CONTROL OF BOTANICALS AND DIETARY SUPPLEMENTS 511
18.7 CONCLUSIONS 512
References 512
Chapter 19 - Analysis of Plant Material 516
19.1 INTRODUCTION 516
19.2 SINGLE DEVELOPMENT 517
19.3 SPECIAL DEVELOPMENT TECHNIQUES 525
19.4 COUPLING PLANAR CHROMATOGRAPHY WITH COLUMN CHROMATOGRAPHY 535
19.5 FORCED-FLOW DEVELOPMENT 535
19.6 CHEMICAL FINGERPRINTING OF PLANT MATERIALS 537
19.7 EFFECT-DIRECTED ANALYSIS OF PLANT MATERIALS 541
19.8 IMAGE PROCESSING 549
References 551
Chapter 20 - Analysis of Dyes and Inks 566
20.1 INTRODUCTION 566
20.2 DYES 568
20.3 INKS 570
20.4 CONCLUSION 594
References 594
Chapter 21 - Analysis of Dietary Supplements 600
21.1 INTRODUCTION 600
21.2 ANALYTICAL CHALLENGES 603
21.3 INSTRUMENTAL TLC 607
21.4 ANALYSIS OF BIOACTIVE INGREDIENTS 617
21.5 FINGERPRINTING AND DETECTION OF ADULTERANTS 638
21.6 CONCLUSIONS 641
References 642
Index 648