High-Speed Countercurrent Chromatography Edited by YOICHIRO ITO Laboratory of Biophysical Chemistry National Institutes of Health Bethesda, Maryland WALTER D. CONWAY Department of Pharmaceutics SUNY Buffalo Buffalo, New York A WILEY-INTERSCIENCE PUBLICATION JOHN WILEY & SONS New York / Chichester / Brisbane / Toronto / Singapore
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High-Speed Countercurrent Chromatography › d315 › 837889d0ba... · 14.3. Analytical Capability of High-Speed Countercurrent Chromatography for Rare Earth Elements 427 14.3.1.
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High-Speed Countercurrent Chromatography
Edited by
YOICHIRO ITO
Laboratory of Biophysical Chemistry National Institutes of Health
Bethesda, Maryland
WALTER D. CONWAY
Department of Pharmaceutics SUNY Buffalo
Buffalo, New York
A WILEY-INTERSCIENCE PUBLICATION
JOHN WILEY & SONS
New York / Chichester / Brisbane / Toronto / Singapore
High-Speed Countercurrent Chromatography
Edited by
YOICHIRO ITO
Laboratory of Biophysical Chemistry National Institutes of Health
Bethesda, Maryland
WALTER D. CONWAY
Department of Pharmaceutics SUNY Buffalo
Buffalo, New York
A WILEY-INTERSCIENCE PUBLICATION
JOHN WILEY & SONS
New York / Chichester / Brisbane / Toronto / Singapore
CONTENTS
PREFACE xvii CUMULATIVE LISTING OF VOLUMES IN SERIES xix
INSTRUMENTATION
CHAPTER 1 PRINCIPLE, APPARATUS, AND METHODOLOGY OF HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY 3 Yoichiro Ito
1.1. Introduction 3 1.2. Principle of High-Speed Countercurrent
Chromatography 5 1.2.1. Two-Phase Distribution in a Rotating
Coil in Unit Gravity 5 1.2.2. Flow-Through Coil Planet Centrifuge
Free of Rotary Seals 11 1.2.3. Mechanism of High-Speed
HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY ON MEDICINAL HERBS 225 Tian- You Zhang
8.1. Introduction 225 8.2. The Present Status of High-Speed
Countercurrent Chromatography on Isolation of Medicinal Herbs 226
8.3. Separations of Substances Prepared From Medicinal Herbs by the Horizontal Flow-Through Coil Planet Centrifuge 227 8.3.1. Apparatus and Experimental
Procedures 227 8.3.2. Separations of a Group of Similar
Substances 228 8.3.3. Studies on the Preparative Capability of
CPC and HPLC in the Separation of Polar Compounds 231
8.4. Separation of Alkaloids, Hydroxyanthraquinones, and Flavonoids by Analytical HSCCC 236 8.4.1. Apparatus and Experimental
Procedures 236 8.4.2. Separation of Alkaloids Extracted from
Stephania tetranda S. Moore 236 8.4.3. Separation of Hydroxyanthraquinone
Derivatives Extracted from Rhubarb 240 8.4.4. Rapid Separation of Flavonoids
Extracted from Sea Buckthorn (Hippophae rhamnoides) 242
8.5. Separations of Flavonoids and Alkaloids by Multilayer Coil Separator and Extractor 245 8.5.1. Apparatus and Experimental
Procedures 245
CONTENTS
8.5.2. Separation of Daphne genkwa Flavonoids 247
8.5.3. Separation of Flavonoids from Crude Extracts of Sea Buckthorn (Hippophae rhamnoides) 249
8.5.4. Separation of Alkaloids from Anisodus tangulicus (Maxin) Pasch 250
8.6. Semipreparative Separation of Alkaloids by GS-10A HSCCC 252 8.6.1. Apparatus and Experimental
Procedures 252 8.6.2. Separation of Alkaloids from
Sophora flavescens Ait and Datura mete L. 252
8.6.3. Separation of Alkaloids from Cephalotaxusfortunei Hook F. 255
8.6.4. Separation of Alkaloids from Senecio fuberi Hemsl 256
8.6.5. Separation of Vincamine and Vincine 259 8.7. Conclusion 262 References 263
CHAPTER 9 ISOLATION OF MARINE NATURAL PRODUCTS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY 265 Nancy L. Fregeau and Kenneth L. Rinehart
9.1. Introduction 265 9.2. Alternative Separation Techniques 267 9.3. Countercurrent Chromatography 268 9.4. Examples of Marine Natural Product Isolations
Using High-Speed Countercurrent Chromatography 268 9.4.1. Macrolides 269 9.4.2. Polyethers 273 9.4.3. Other Acetate-Derived Metabolites 275 9.4.4. Terpenes and Steroids 276 9.4.5. Peptides 278 9.4.6. Nitrogen-Containing Heterocycles 280
9.5. Conclusion 296 References 297
CONTENTS Xll l
CHAPTER 10 SEPARATION OF COMPLICATED ANTIBIOTICS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY 301 Ken-Ichi Harada
10.1. Introduction 301 10.2. Selected Antibiotics 302 10.3. Operation of HSCCC 304 10.4. Establishment of HPLC for SVD and BC 304 10.5. Selection of Proper Two-Phase Solvent
System 307 10.6. Separation of SVD and BC Components by
HSCCC 314 10.7. Comparison of Elution Behavior of SVD and
BC between HPLC and HSCCC 314 10.8. Conclusion 317 References 318
CHAPTER 11 N-BROMOACETYL-3,3 5-TRIIODO-L-THYRONINE AND JV-BROMOACETYL-L-THYROXINE: SYNTHESIS AND CHARACTERIZATION 321 Hans J. Cahnmann
11.1. 11.2.
11.3.
11.4.
11.5. Refe
Introduction Synthesis 11.2.1. Synthesis of BrAcT3
Verification of Identity and Purity 11.4.1. HPLC 11.4.2. TLC 11.4.3. Absorption Spectra in the Near UV Summary
rences
321 322 324 325 326
326 328 330 330
330 331 331 331 333 334 335
XIV CONTENTS
CHAPTER 12 SEPARATION AND PURIFICATION OF DYES BY CONVENTIONAL HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY AND pH-ZONE-REFINING COUNTERCURRENT CHROMATOGRAPHY 337 Adrian Weisz
KTand KE 419 14.2.5. Partition Efficiencies 422 14.2.6. Gradient Elution of Fourteen Rare
Earth Elements 426 14.3. Analytical Capability of High-Speed
Countercurrent Chromatography for Rare Earth Elements 427 14.3.1. Reproducibility of Chromatogram 428 14.3.2. Quantitative Determination of Cerium
Impurities in Erbium Chloride 430 14.4. Separation of Other Inorganic Elements by
High-Speed Countercurrent Chromatography 430 14.4.1. Separation of Ortho-and
Pyrophosphate Ions 431 14.4.2. Separation of Cesium and Strontium 432 14.4.3. Separation of Zirconium and Hafnium 432 14.4.4. Separation of Cadmium and Zinc 435 14.4.5. Separation of Nickel, Cobalt,
Magnesium, and Copper 435 14.4.6. Separation of Copper, Cadmium, and
Manganese 437 14.4.7. Separation of Iron(II) and Iron(III) 438 14.4.8. Preconcentration of Trace Elements
from Certain Rock Macrocomponents 438 References 441