Protein Structure Chasman

Preparative Layer Chromatography......Page 6
Preface......Page 8
About the Editors......Page 9
Contributor List......Page 11
Contents......Page 13
Table of Contents......Page 0
Section I......Page 15
1.1 CHROMATOGRAPHY BACKGROUND......Page 16
1.2 BASICS OF PLC......Page 17
1.3 PRINCIPLES AND CHARACTERISTICS OF PLC......Page 18
1.4 ORGANIZATION OF THE BOOK......Page 21
REFERENCES......Page 23
CONTENTS......Page 24
2.1 ADSORPTION ON A SOLID–LIQUID INTERFACE AND THE EXPERIMENTAL ISOTHERMS OF ADSORPTION......Page 25
2.2 TLC IN THE LINEAR AND THE NONLINEAR REGION OF THE ADSORPTION ISOTHERM......Page 29
2.3 PREPARATIVE LAYER CHROMATOGRAPHY AS A PRACTICAL USAGE OF THE NONLINEAR REGION......Page 34
2.4 LATERAL INTERACTIONS AND THEIR IMPACT ON SEPARATION IN PLC......Page 35
2.4.1.2 alpha,Omega-Dicarboxylic Acids......Page 37
2.4.1.3 Phenyl-Substituted Monocarboxylic Acids......Page 39
2.4.2 MIXED-ASSOCIATIVE LATERAL INTERACTIONS......Page 41
2.4.3 LATERAL INTERACTIONS IN THE RACEMIC MIXTURES......Page 44
2.5 THE MEANING OF THE RETARDATION FACTOR (RF) IN PLC......Page 45
2.6.1 THE MASS-TRANSFER EQUATIONS......Page 47
2.6.2 MODELING OF THE SELF-ASSOCIATIVE LATERAL INTERACTIONS......Page 48
2.6.3 MODELING OF MIXED-ASSOCIATIVE LATERAL INTERACTIONS......Page 50
REFERENCES......Page 52
3.1 SORBENT MATERIALS AND PRECOATED LAYERS FOR STRAIGHT PHASE CHROMATOGRAPHY......Page 54
3.1.1 SILICA GEL BULK MATERIALS......Page 55
3.1.2 SILICA GEL PRECOATED PLATES......Page 56
3.1.4 ALUMINUM OXIDE PRECOATED PLATES......Page 64
3.2.1 SILICA GEL......Page 67
3.2.3 CELLULOSE......Page 68
3.3 PRECOATED LAYERS FOR REVERSED-PHASE CHROMATOGRAPHY......Page 69
REFERENCES......Page 71
4.1 INTRODUCTION......Page 74
4.2 SELECTION OF MOBILE PHASE......Page 77
4.2.1 REQUIREMENTS FOR THE MOBILE PHASE......Page 78
4.2.2 INFLUENCE OF THE STATIONARY PHASE......Page 79
4.2.3 PROPERTIES OF SOLVENTS......Page 81
4.2.4 SOLVENT CLASSIFICATION IN ELUOTROPIC SERIES......Page 87
4.2.5 SNYDER’S SOLVENT CLASSIFICATION......Page 92
4.2.6 SOLVATOCHROMIC CLASSIFICATION......Page 94
4.2.7 PRELIMINARY WORK FOR MOBILE PHASE SELECTION......Page 96
4.2.7.2 Selection by Solvent Character......Page 97
4.2.7.3 Selection by Selectivity and Strength of Solvent......Page 99
4.3.1 THERMODYNAMIC MODEL......Page 100
4.3.2 SNYDER–SOCZEWINSKI MODEL......Page 102
4.3.3 PRISMA MODEL......Page 103
4.3.4 WINDOW DIAGRAM METHOD......Page 105
4.3.5 COMPUTER-ASSISTED METHODS......Page 106
4.4 CONCLUSION......Page 107
REFERENCES......Page 108
CONTENTS......Page 112
5.1 SAMPLE APPLICATION......Page 113
5.1.1.2 Property of the Sample Solvent......Page 114
5.1.1.3 Concentration of the Solution......Page 115
5.1.2 APPLICATION PATTERN......Page 116
5.1.3.1 Manual Application and Focusing......Page 117
5.1.3.2 Automated Application......Page 119
5.1.3.2.1 Semiautomatic Application......Page 120
5.1.3.2.2 Fully Automated Application......Page 123
5.1.3.3 Solid Phase Sample Application (SPSA)......Page 124
5.2.2 PREWASHING OF PREPARATIVE LAYERS......Page 126
5.2.2.1 Techniques of Prewashing......Page 128
5.2.2.2 Drying and Storage of Prewashed Plates......Page 130
5.2.3.1 Handling of the Mobile Phase......Page 132
5.2.3.2 Separation Techniques......Page 133
5.2.3.3 Separation Chambers......Page 134
5.2.3.4 Drying of Developed Plates......Page 136
5.2.4 INFLUENCING FACTORS — CHAMBER CLIMATE......Page 137
5.2.4.1 Unsaturated Chamber......Page 138
5.2.4.2 Chamber Saturation......Page 139
5.2.4.3 Conditioning of the Layer Just before Chromatography......Page 140
5.2.4.4 Sandwich Configuration......Page 141
REFERENCES......Page 142
CONTENTS......Page 144
6.2 CHAMBER TYPES......Page 145
6.2.1 HORIZONTAL CHAMBERS FOR LINEAR DEVELOPMENT......Page 146
6.2.2 HORIZONTAL CHAMBERS FOR RADIAL DEVELOPMENT......Page 151
6.3.1.1 Isocratic Linear Development......Page 153
6.3.1.2 Continuous Isocratic Development......Page 154
6.3.1.3 Short Bed–Continuous Development......Page 155
6.3.1.4 Two-Dimensional Separations......Page 157
6.3.1.6 Gradient (Stepwise and Continuous) Development......Page 158
6.3.1.8 Temperature Control......Page 161
6.3.2.1 Circular Development......Page 162
6.3.2.2 Anticircular Development......Page 164
6.3.3.1 Preconcentration......Page 166
6.3.3.3 Band Application......Page 169
6.4 REGENERATION OF THE LAYERS......Page 172
REFERENCES......Page 173
7.1 INTRODUCTION......Page 175
7.2 THE KUBELKA–MUNK THEORY OF REMISSION......Page 176
7.2.1 DIRECT DETECTION IN ABSORPTION......Page 178
7.2.2 DIRECT DETECTION IN FLUORESCENCE......Page 179
7.2.3 FLUORESCENCE QUENCHING......Page 181
7.3.1 NONDESTRUCTIVE DYEING (BY IODINE VAPOR AND WATER)......Page 182
7.3.2 FLUORESCENCE AND PH REAGENTS......Page 183
7.3.3 UNIVERSAL DETECTION REAGENTS (CHARRING)......Page 184
7.3.4 SELECTIVE DETECTION REAGENTS......Page 185
REFERENCES......Page 186
8.1 INTRODUCTION......Page 188
8.2.3.1 Contact Film Autoradiography......Page 191
8.2.4 BIOLOGICAL DETECTION......Page 192
8.3 REMOVAL OF SUBSTANCES FROM THE LAYER......Page 194
8.4 RECENT APPLICATIONS OF PLC......Page 197
REFERENCES......Page 198
Section II......Page 201
9.1 INTRODUCTION......Page 202
9.2 BIOLOGICAL MATRICES AND THEIR COMPONENTS......Page 203
9.2.1 SHORT CHARACTERISTICS OF THE MATRICES......Page 204
9.2.2.3 Lipids......Page 205
9.2.2.5 Drugs......Page 206
9.3 SEPARATION AND DESORPTION TECHNIQUES......Page 207
9.3.1 SPECIFICITY OF CHROMATOGRAPHIC SYSTEMS......Page 208
9.3.2 REMOVAL AND RECOVERY OF SUBSTANCES FROM THE LAYER......Page 211
9.4 APPLICATIONS......Page 219
9.4.1 AMINO ACIDS AND PEPTIDES......Page 220
9.4.2 CARBOHYDRATES......Page 221
9.4.3 LIPIDS......Page 224
9.4.4 BILE ACIDS......Page 227
9.4.5 PHARMACOKINETIC AND TOXICOLOGICAL STUDIES OF DRUGS......Page 230
9.4.6 RESEARCH OF ENZYME ACTIVITIES......Page 236
9.4.7 OTHER APPLICATIONS......Page 239
REFERENCES......Page 241
10.1 INTRODUCTION......Page 246
10.3 RIBOFLAVIN (VITAMIN B2)......Page 247
10.4 PYRIDOXINE (VITAMIN B6)......Page 248
10.5 COBALAMIN (VITAMIN B12)......Page 249
10.7 PANTOTHENIC ACID......Page 251
10.9 FOLIC ACID......Page 253
10.10 ASCORBIC ACID (VITAMIN C)......Page 255
REFERENCES......Page 259
CONTENTS......Page 260
11.2 GOALS OF PREPARATIVE LAYER CHROMATOGRAPHY OF PLANT EXTRACTS......Page 261
11.2.2 PLC AS A METHOD OF SAMPLE PREPARATION......Page 262
11.2.3 PLC AS A PILOT TECHNIQUE FOR PREPARATIVE COLUMN CHROMATOGRAPHY......Page 265
11.3 GENERAL PRINCIPLES OF THE CHOICE OF CHROMATOGRAPHIC SYSTEMS IN PLC OF PLANT EXTRACTS......Page 268
11.3.1 APPLICATION OF DIFFERENT SELECTIVITY SYSTEMS FOR THE SEPARATION OF CLOSELY RELATED COMPOUNDS......Page 278
11.4.1 KIND OF OVERLOADING......Page 285
11.4.2 SAMPLING MODE......Page 287
11.5 INFLUENCE OF SAMPLE SOLVENTS ON FORMATION AND MIGRATION OF ZONES......Page 290
11.6 DIFFERENT TYPES OF DETECTION IN PLC OF NATURAL MIXTURES......Page 293
11.7 SPECIAL MODES OF DEVELOPMENT AS A TOOL IN PREPARATIVE SEPARATION OF PLANT EXTRACTS......Page 294
11.7.1 GRADIENT ELUTION......Page 295
11.7.2 UNIDIMENSIONAL MULTIPLE DEVELOPMENT (UMD)......Page 297
11.7.3 INCREMENTAL MULTIPLE DEVELOPMENT (IMD)......Page 299
11.7.4 TWO-DIMENSIONAL TLC IN PREPARATIVE SCALE......Page 300
REFERENCES......Page 303
CONTENTS......Page 308
12.2 BASIC STRUCTURES AND NOMENCLATURE OF SIMPLE AND COMPLEX LIPIDS......Page 309
12.2.1.3 Acylglycerols......Page 310
12.2.1.4 Sterols and Their Esters......Page 311
12.2.2.2 Glycolipids......Page 312
12.4.1 SOLID PHASE OR ADSORBENTS AND SELECTION OF THE STATIONARY PHASE......Page 313
12.4.2 MOBILE PHASES AND SELECTION OF A SOLVENT SYSTEM......Page 314
12.4.3 PREPARATION OF LIPID/OIL SAMPLES FOR PLC: IMPORTANCE OF THE CONCENTRATION AND DISSOLVING SOLVENT......Page 315
12.4.4 SAMPLE APPLICATION: METHODS OF APPLICATION, MANUAL AND INSTRUMENTAL, SAMPLE LOAD......Page 316
12.4.5 DEVELOPMENT AND CHAMBER TYPES......Page 317
12.4.6.2 Solvent Systems......Page 318
12.4.7.1.1 Simple Lipids......Page 319
12.4.7.2.1 Simple and Phospholipids......Page 321
12.4.7.2.2 Gangliosides and Glycolipids......Page 322
12.4.8.2 Other Detection Methods......Page 323
12.5.1 MEDICINE AND PHARMACOLOGICAL RESEARCH AND DRUGS......Page 327
12.5.3 BIOLOGY AND BIOCHEMISTRY......Page 328
REFERENCES......Page 331
CONTENTS......Page 334
13.1.1 PIGMENT CLASSES......Page 335
13.2.1 STATIONARY PHASES......Page 336
13.2.3 RECOVERY OF SEPARATED COMPONENTS......Page 338
13.3.2 SOURCES AND DISTRIBUTION......Page 339
13.3.4 PRACTICAL PROCEDURES......Page 341
13.4.1 STRUCTURES......Page 343
13.4.3 CHOICE OF SYSTEMS FOR SEPARATION......Page 344
13.4.4 PRACTICAL PROCEDURES......Page 345
13.5.2 SOURCES AND DISTRIBUTION......Page 346
13.5.4 PRACTICAL PROCEDURES......Page 347
13.6.1 STRUCTURES......Page 348
13.6.4 PRACTICAL PROCEDURES......Page 349
13.7.1 STRUCTURES......Page 350
13.7.4 PRACTICAL PROCEDURES......Page 351
13.8.2 SOURCES AND DISTRIBUTION......Page 352
REFERENCES......Page 353
14.1 INTRODUCTION......Page 356
14.2 METHODOLOGY......Page 358
14.3 SAMPLE PREPARATION......Page 359
14.4 STATIONARY PHASE......Page 360
14.6 DETECTION AND IDENTIFICATION......Page 361
14.7 QUANTIFICATION......Page 362
14.8.2 ANALYSIS OF FOOD SAMPLES......Page 363
14.8.3.1 Analysis of Rocks and Minerals......Page 367
14.8.3.2 Analysis of Monazite Sand......Page 368
14.8.4 ANALYSIS OF ALLOYS......Page 369
14.8.8.1 Human Placenta Sample......Page 370
14.8.8.2 Human Viscera Sample......Page 372
ACKNOWLEDGMENT......Page 374
REFERENCES......Page 375
15.1 INTRODUCTION......Page 378
15.2.2 COLUMN CHROMATOGRAPHY IN SOLUBLE ORGANIC MATTER FRACTIONATION......Page 380
15.2.3 PTLC IN GROUP COMPOSITION INVESTIGATION......Page 382
15.3.1 FRACTIONATION OF AROMATIC COMPOUNDS......Page 386
15.3.2 SULFUR COMPOUND SEPARATION......Page 387
15.3.3 POLAR COMPOUNDS FRACTIONATION......Page 388
15.4 WHAT GEOCHEMICAL INFORMATION PLC RESULTS YIELD AND HOW TO INTERPRET THEM......Page 390
15.4.2 EXPULSION TYPE......Page 391
15.4.3 THERMAL MATURITY......Page 392
15.4.5 BIODEGRADATION......Page 393
15.5 CONCLUSIONS......Page 394
REFERENCES......Page 395
CONTENTS......Page 400
16.1 OLIBANUM RESINS......Page 401
16.2.2 COMPARISON OF THE RESULTS OBTAINED BY GC–MS TO THOSE OBTAINED BY TLC......Page 402
16.3.2.1 Isolation of Verticilla-4(20),7,11-Triene (Compound 1)......Page 406
16.3.3.2 Isolation of Cembrenol (Compound 6)......Page 410
16.4.2 SELECTION AND SEPARATION OF THE PYROLYZED TRITERPENES......Page 412
16.4.2.1 Separation of the Nortriterpenes with Carbohydrate Structure of B. carterii......Page 413
16.4.2.2 Separation and Isolation of an Oxidized Notriterpene of B. serrata......Page 414
16.5 DETERMINATION OF TWO BOSWELLIC ACIDS AS MARKER OF ALTERATIONS DURING PROCESSING OF THE RESINS......Page 415
16.6 GENERAL ISOLATION INSTRUCTIONS......Page 417
REFERENCES......Page 419