Countercurrent chromatography: the support-free liquid stationary phase
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Format: | Buch |
---|---|
Sprache: | English |
Veröffentlicht: |
Boston, Mass.
Elsevier
2002
|
Ausgabe: | 1. ed. |
Schriftenreihe: | Wilson and Wilson's Comprehensive analytical chemistry
38 |
Schlagworte: | |
Online-Zugang: | Inhaltsverzeichnis |
Beschreibung: | Includes bibliographical references and index. - Erscheint: September 2002 |
Beschreibung: | XXIV, 397 S. Ill., graph. Darst. |
ISBN: | 044450737X |
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245 | 1 | 0 | |a Countercurrent chromatography |b the support-free liquid stationary phase |c ed. by Alain Berthod |
250 | |a 1. ed. | ||
264 | 1 | |a Boston, Mass. |b Elsevier |c 2002 | |
300 | |a XXIV, 397 S. |b Ill., graph. Darst. | ||
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Datensatz im Suchindex
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adam_text | Titel: Countercurrent chromatography
Autor: Berthod, Alain
Jahr: 2002
Contents
Foreword....................................xix
Series Editor s Preface.............................xxi
Preface.....................................xxiii
Chapter 1. Fundamentals of countercurrent chromatography..............1
Alain Berthod
1.1 Introduction..........................1
1.2 A liquid stationary phase...................1
1.3 Chromatographic theory...................2
1.3.1 Fundamental retention equation..........2
1.3.2 Retention factor and selectivity..........4
1.3.3 Resolution......................5
1.4 CCC and HPLC........................8
1.4.1 Plate count working range.............8
1.4.2 CCC is fundamentally a preparative technique . 10
1.4.3 Two complementary techniques.........12
1.5 Hydrodynamic and hydrostatic CCC columns.......12
1.5.1 Hydrodynamic CCC columns...........13
1.5.2 Hydrostatic CCC columns.............15
1.5.3 Pressure drop in CCC machines.........18
1.6 Conclusion..........................19
References...............................19
Chapter 2. Operating a countercurrent chromatography machine..........21
Alain Berthod, Les Brown, Gilda G. Leitao and Suzana G. Leitao
2.1 Introduction.........................21
2.2 Liquid system preparation..................22
2.2.1 Basic properties of ternary phase diagrams ... 22
2.2.2 Liquid system equilibrium............24
2.2.3 Effect of temperature...............25
2.3 Apparatus preparation....................25
2.3.1 Classical column preparation..........25
2.3.2 Direct injection..................26
xi
2.3.3 Sample injection..................26
2.3.4 Column stability..................27
2.4 Effect of machine specifications on separations.......27
2.4.1 Effect of the stationary-phase volume......28
2.4.2 Machine transposition...............30
2.5 Working with a wide polarity range.............33
2.5.1 Introduction....................33
2.5.2 The dual-mode CCC chromatogram.......34
2.5.3 Emptying a machine................36
2.5.4 Gradient elution..................37
2.6 Two practical examples...................40
2.6.1 Purification of active alkaloids from a Brazilian
plant extract....................40
2.6.2 From a crude plant-extract to pure flavonoids
in two CCC steps..................42
2.7 Conclusion..........................46
References...............................46
Chapter 3. Solvent systems.........................................49
Jean-Hugues Renault, Jean-Marc Nuzillard, Olivier Intes and
Alexandre Maciuk
3.1 Introduction.........................49
3.2 Generalities on biphasic solvent systems..........50
3.3 Strategies for solvent-system selection...........54
3.3.1 General comments.................54
3.3.2 The best solvent approach...........54
3.3.3 Multisolvent system approach..........63
3.3.4 Biphasic aqueous-aqueous solvent systems ... 68
3.3.5 A practical approach to the selection of solvent
systems.......................69
3.4 From an empty box to a fit column.............69
3.4.1 Generalities....................69
3.4.2 Chemical structures as a starting point.....71
3.5 Conclusion..........................81
References...............................81
Chapter 4. Centrifugal partition chromatography: the story of a company ... 85
Alain P. Foucault
4.1 Introduction.........................85
4.2 The story of CPC.......................85
4.2.1 The roots......................85
4.2.2 The first paper...................87
4.2.3 Change of name from CCCC-RJ to CPC.....88
4.2.4 The CPC-LLN...................90
xii
4.2.5 The HPCPC series 1000.............. 95
4.2.6 Large-scale instruments.............101
4.3 Newcomers and new approaches..............105
4.3.1 The Dutch School................105
4.3.2 The French School................107
4.4 Future trends........................Ill
References..............................Ill
Chapter 5. Centrifugal partition chromatography: an engineering
approach....................................................115
Luc Marchal, Alain P. Foucault, Gerard Patissier, Jean-Michel Rosant
and Jack Legrand
5.1 Introduction.........................115
5.2 Assumptions and first visualizations............116
5.2.1 The first image of CPC..............116
5.2.2 Van Deemter-type plots and the three-stage
model.......................117
5.2.3 The Stokes model.................119
5.2.4 The first visual and chemical engineering
approach: the Dutch school...........121
5.3 Chromatography curves model...............122
5.3.1 Chromatography theory.............122
5.3.2 The CPC model..................129
5.4 Flow patterns, residence time distribution and mass
transfer...........................131
5.4.1 Experimental...................131
5.4.2 Review of the different types of flow-regimes. . 135
5.4.3 Flow patterns in CPC..............137
5.4.4 Residence time distribution...........145
5.4.5 Mass transfer...................148
5.4.6 Efficiency and resolution.............151
5.5 Conclusion..........................155
References..............................156
Chapter 6. Liquid stationary phase retention and resolution in
hydrodynamic CCC...........................................159
Ian A. Sutherland
6.1 Introduction.........................159
6.2 Head/tail rule........................161
6.3 Measuring dead volume (Vd) and retention of the
stationary phase (S/) in the coil planet centrifuge.....161
6.4 Predicting peak elution...................166
6.4.1 Elution of solvent front (Kn = 0)........166
6.4.2 Elution of Kn = 1 Peak..............166
6.4.3 Elution of a solute with distribution ratio (KD). 167
6.5 Modelling CCC using an eluting CCD model.......168
6.6 Practical application of the model.............171
6.7 Conclusions.........................175
References..............................175
Chapter 7. Special uses of a support-free liquid stationary phase..........177
Beatrice Billardello and Alain Berthod
7.1 Introduction.........................177
7.2 Displacement chromatography...............177
7.2.1 Principle.....................177
7.2.2 A practical example: separating cations.....178
7.3 pH-Zone refining......................181
7.3.1 Principle.....................181
7.3.2 Simple modelling of the phenomenon......183
7.3.3 Modelling zone formation............184
7.3.4 Hydrophobicity versus acid strength: case
study of zone overlap...............186
7.4 Liquid-liquid partition coefficient determination.....192
7.4.1 Direct measurement of liquid-liquid
distribution constants..............192
7.4.2 Dual-mode CCC.................193
7.4.3 Other liquid-liquid distribution coefficient
measurements..................194
7.5 Other uses of the liquid nature of the stationary phase. . 195
7.5.1 Continuous extraction..............195
7.5.2 Rapid determination of liquid-liquid isotherms 196
7.5.3 A liquid-liquid reactor for catalytic reactions. . 197
7.6 Conclusion..........................198
References..............................199
Chapter 8. Separation and purification of natural products (medicinal
herbs) by high speed countercurrent chromatography................201
Tianyou Zhang
8.1 Introduction.........................201
8.2 Apparatus for high-speed CCC...............202
8.2.1 Semi-preparative HSCCC............202
8.2.2 Analytical HSCCC................203
8.2.3 Two-dimensional HSCCC system........203
8.2.4 pH-Zone-refining CCC system..........204
8.2.5 Cross-axis CCC..................205
8.3 Applications of semi-preparative HSCCC.........206
8.3.1 Separation of 10-deacetylbaccatin III from the
needles of Taxus chinensis............206
xiv
8.3.2 Separation of a stilbene glycoside from
Polygonum multiflorum Thunb.........209
8.3.3 Separation of Resveratrol and Piceid from
extract of Polygonum cuspidatum Sieb. et Zucc 214
8.3.4 Separation of gallic acid from Cornus officinalis
Sieb. et Zucc...................215
8.4 Applications of analytical HSCCC.............218
8.4.1 Separation of Alkaloids from Coptis chinensis
Franch......................218
8.4.2 Separation of isoflavones from Pueraria lobata
(willd.) Ohwi...................223
8.4.3 Separation of catechins from tea polyphenols . 226
8.4.4 Separation of notopterol and isoimperatorin
from Notopterygium forbessi Boiss.......233
8.4.5 Separation of tanshinones from Salvia
miltiorrhiza Bunge................239
8.5 Application of two-dimensional HSCCC systems.....244
8.5.1 Separation of flavone aglycones from
Hippophae rhamnoids L..............244
8.5.2 Separation of flavone aglycones from the
leaves of Ginkgo biloba L............246
8.6 Applications of the pH-zone-refining CCC system.....247
8.6.1 Preparative separation of alkaloids from the
root of Sophora flavescens Ait..........247
8.6.2 Preparative separation of lappaconitine by
pH-zone-refining CCC..............251
8.7 Applications for a cross-axis CCC machine........254
8.7.1 Partition of protein in aqueous two-phase
systems......................254
8.7.2 Standard proteins separation..........255
8.7.3 Preparation of glycoprotein from Morchella
esculenta (L.)...................256
8.8 Conclusion..........................258
References..............................259
Chapter 9. Separation of inorganic compounds: theory, methodology and
applications.................................................261
Yu-Ren Jin, Li-Xing Zhang, Lian-Zhong Zhang and Shi-Jun Han
9.1 Introduction.........................261
9.2 Theory............................262
9.2.1 Definitions and expressions...........262
9.2.2 Retention of inorganic compounds.......263
9.2.3 Separation efficiency...............270
9.3 Methodology.........................276
xv
9.3.1 Experimental procedure.............277
, . 9.3.2 Elution mode...................273
9.3.3 Two-phase system................277
9.3.4 Operational parameters.............232
9.4 Applications.........................273
9.4.1 Preconcentration of metal ions.........2.ro
9.4.2 Determination of plutonium in soil by
ICP-MS after CCC pre-separation........291
9.5 Summary..........................297
References..............................297
Chapter 10. The use of CCC in the pharmaceutical industry.............30 i
Guy H. Harris
10.1 Introduction.........................301
10.2 The use of CCC for natural product crude extract
fractionation.........................302
10.2.1 The problem...................302
10.2.2 CCC as a solution: methodology and solvent
, systems for crude extracts............303
10.2.3 CCC as a general first isolation step for natural
product extracts—examples...........306
10.2.4 Application of CCC to crude extract
pre-fractionation for bioassay—examples. . . . 314
10.2.5 Application of CCC to the deconvolution of
combinatorial libraries..............317
10.3 The use of CCC for bioassay-guided isolation of natural
products...........................317
10.3.1 Bioassay-guided isolation of natural products
using CCC....................317
10.3.2 Application of CCC to bioassay-guided isolation
problems—examples...............318
10.4 Industrial scaleup of CCC..................325
10.5 Future directions......................327
Acknowledgements.........................328
References..............................328
Chapter 11. Enantioseparations in countercurrent chromatography and
centrifugal partition chromatography............................331
Laureano Oliveros, Cristina Minguillon, Pilar Franco and
Alain P. Foucault
11.1 Introduction.........................331
11.2 Chiral separations......................332
11.3 Chiral CCC: the pioneers..................334
11.4 N-Dodecanoyl-L-proline-3,5-dimethylanilide.......335
11.4.1 Following the Pirkle path............335
xvi
11.4.2 Chiral separation by pH-zone refining.....337
11.5 Sulfated [3-cyclodextrin...................339
11.6 Bovine serum albumin (BSA)................341
11.7 Vancomycin.........................343
11.8 Cinchona alkaloid derivatives...............344
11.9 Chiral CCC reactor.....................345
11.10 Conclusion..........................349
References..............................349
Chapter 12. Supercritical fluids as mobile phases in CCC...............353
Tiing Yu and Yu Chuan Chen.......................353
12.1 Introduction.........................353
12.1.1 Definition of supercritical fluids.........353
12.1.2 Applications of supercritical fluid
chromatography and extraction.........354
12.1.3 Supercritical fluids as mobile phase in CCC . . 355
12.2 Experimental apparatus and procedures.........356
12.2.1 Experimental set-ups..............356
12.2.2 Experimental procedures............358
12.3 Separation of some small organic compounds.......360
12.3.1 The first chromatograms............360
12.3.2 Temperature effect on separation resolution . . 362
12.3.3 Pressure effect on separation resolution .... 364
12.3.4 Stationary phase composition effect on
separation resolution...............364
12.4 Separation of steroids....................365
12.5 Supercritical fluid extraction using a CCC apparatus. . . 368
12.5.1 Theory......................368
12.5.2 Results......................372
12.6 Conclusions and perspectives................375
Acknowledgement..........................375
References..............................376
Appendix. Commercially available countercurrent chromatographs.......379
Alain Berthod...............................379
A.l Twentieth century CCC technology............379
A.l.l Discontinued apparatuses............379
A.l.2 Hydrostatic machines..............380
A.2 Twenty-first century CCC machines............381
A.2.1 Hydrodynamic machines.............381
A.2.2 Hydrostatic machines..............386
Glossary.......................................................389
Index.........................................................393
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isbn | 044450737X |
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physical | XXIV, 397 S. Ill., graph. Darst. |
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spelling | Countercurrent chromatography the support-free liquid stationary phase ed. by Alain Berthod 1. ed. Boston, Mass. Elsevier 2002 XXIV, 397 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Wilson and Wilson's Comprehensive analytical chemistry 38 Includes bibliographical references and index. - Erscheint: September 2002 Gegenstromchromatographie (DE-588)4241437-4 gnd rswk-swf Gegenstromchromatographie (DE-588)4241437-4 s DE-604 Berthod, Alain Sonstige oth Wilson and Wilson's Comprehensive analytical chemistry 38 (DE-604)BV000900805 38 HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=009920503&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
spellingShingle | Countercurrent chromatography the support-free liquid stationary phase Wilson and Wilson's Comprehensive analytical chemistry Gegenstromchromatographie (DE-588)4241437-4 gnd |
subject_GND | (DE-588)4241437-4 |
title | Countercurrent chromatography the support-free liquid stationary phase |
title_auth | Countercurrent chromatography the support-free liquid stationary phase |
title_exact_search | Countercurrent chromatography the support-free liquid stationary phase |
title_full | Countercurrent chromatography the support-free liquid stationary phase ed. by Alain Berthod |
title_fullStr | Countercurrent chromatography the support-free liquid stationary phase ed. by Alain Berthod |
title_full_unstemmed | Countercurrent chromatography the support-free liquid stationary phase ed. by Alain Berthod |
title_short | Countercurrent chromatography |
title_sort | countercurrent chromatography the support free liquid stationary phase |
title_sub | the support-free liquid stationary phase |
topic | Gegenstromchromatographie (DE-588)4241437-4 gnd |
topic_facet | Gegenstromchromatographie |
url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=009920503&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
volume_link | (DE-604)BV000900805 |
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