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1 232 U.S. Food and Drug Administration, 156,184,203,218 Université de Lausanne, 143 Université de Lyon 1, 16 MODERN COUNTERCURRENT CHROMATOGRAPHY University of Illinois at Urbana- Champaign, 129 Upjohn Laboratories, 78 Subject Index Downloaded via on August 20, 2018 at 05:59:35 (UTC). See for options on how to legitimately share published articles. A Acetyltylophoroside, purification by 85 Acquired immunodeficiency syndrome (AIDS),drug directed at reverse transcriptase enzyme, 111 Alkaloids, separation from Senecio fuberi Hemsl chromatography, applications, 91 buffer ph vs. retention, 88,91 chromatograms, 88,90/ experimental procedure, TLC analysis of fractions, 88,90/ Ammonia, concentration in mobile phase, effect on CCC of, 226,227/ Apparent partition coefficient of retainer acid, calculation, Apparent solute partition coefficient, calculation, 165,167 Aqueous alcohol-hydrocarbon solvent systems, optimization, 80 Aspartyl proteinase substrate peptide, purification, Β Bond number values, 69-71/ C Centrifugal partition chromatography flow pattern model of mobile phase, partition coefficient measurement, Chambered plate chromatography, description, 5,8/ Coil planet centrifuge cross-axis, use of experimental design to determine optimal settings, description, 4-6/ type J, comparison using orbital turns per theoretical plate, Coil planet centrifuge chromatography, liquid flow, 5,7,8/ Count of orbital rounds per plate, definition, 37 Countercurrent chromatography advantages, 11,13,78,156 applications, 1-2 chambered plate chromatographs, 5,8/ coil planet centrifuges, 4-6/ comparison to other chromatographies, 2 description, 218 droplet 4,6/ examples of coupled MS techniques, high- and low-density lipoprotein fractions from human serum, isolation, high speed, See High-speed countercurrent chromatography history, 3-4 instrumentation, 129 isolation of high- and low-density lipoprotein fractions from human serum, mobile phase, 16 modern apparatus, 4-6/8/ optimization of solvent systems, overview, 1-13 partition coefficient, 2

2 INDEX 233 Countercurrent chromatography Continued chromatography, 10-12/ purification of HTV-1 aspartyl proteinase substrate peptide, preparative technique, 3 sample recovery, 3 separation of alkaloids from Senecio fuberi, separation of cucurbitacin Β and Ε from fruit base of Cucumis melo, separation of gardenia yellow components, solvent systems, 10 stationary-phase retention, theory, 7,9-10,12/ types, Countercurrent distribution model mass balance equation, 185,187 procedure, 185,186/ Crocin, separation by high-speed Cross-axis coil planet centrifuge, use of experimental design to determine optimal settings, Cucumis melo L., separation of cucurbitacin Β and Ε from fruit base chromatography, Cucurbitacin Β and E, separation from fruit base of Cucumis melo L. by high-speed apparatus, 107 chromatogram, 108,110/ experimental procedure, 107 HPLC analysis, 108,109/ D D&C Orange No. 5, ph-zone-refining / Dinitrophenylamino acids, chromatography, Dipeptides, on-line FAB MS detection in high-speed countercurrent chromatography through moving belt interface, Diprotic acid, ph-zone-refining Dispersion term, 66,69-71/ Displacement chromatography, comparison to chromatography, 178, Droplet description, 4,6/ Ε Effective section, definition, 37 Eluent base concentration, component purification, 226, Elution rate of trailing border of retainer acid, calculation, Equilibrium model for ph-zone-refining countercurrent distribution model, diprotic acid, mathematical solution, 187 monoprotic acid mixture, 194,196/ plateau concentration of monoprotic acid, 197 plateau ph prediction, 194, retaining acid effect, Erythromycins, on-line FAB MS detection in high-speed countercurrent chromatography through moving belt interface, Ethyl acetate-hexane-aqueous methanol systems, optimization, 80 Experimental design to determine optical settings of cross-axis coil planet centrifuge, advantages, graphical analysis, interpretation by solvent, interpretation methods, 56,60 methodology, 50-53

3 234 MODERN COUNTERCURRENT CHROMATOGRAPHY Experimental design to determine optical settings of cross-axis coil planet centrifuge Continued overall interpretation, 50,54 solvents, Fast atom bombardment MS detection in high-speed countercurrent chromatography through moving belt interface, on line, Flow pattern of mobile phase in centrifugal partition chromatography, model based on Stokes law, apparatus, bond number, 69-71/ consequence of Stokes' model, 70,72-74/ dispersion term, 66,69-71/ experimental procedure, 63 interfacial area between phases in channels, 70,72 linear velocities and diameter of Stokes droplets, 64,66i linear velocity-flow rate relationship, mobile-phase volume-flow rate relationship, 63-64,67/ mobile-phase volume-rotational speed relationship, 66,67-68/ systems used, 64,65f Fractional volume of column occupied by stationary phase, definition, Fruit base of Cucumis melo L., separation of cucurbitacin Β and Ε chromatography, G Gardenia yellow components, separation chromatography, experimental procedure, HPLC identification, / photoisomerization of crocin, 105 Gardenia yellow components, separation chromatography Continued purification, 102,104/ selection of two-phase solvent system, 95, i Geniposide, separation by high-speed Guadi, separation of cucurbitacin Β and Ε chromatography, Η Halocarbon-aqueous methanol systems, optimization, 80 Heptane-water systems, partition coefficients, 151 Hexane-aqueous methanol systems, optimization, 80 High- and low-density lipoprotein fractions from human serum, isolation by apparatus, composition of aqueous polymer phase systems, 120,121/ experimental procedure, flow rate, 125,126/ partition coefficients of lipoproteins and serum proteins, 123,124/ polyacrylamide gel electrophoresis of fractions, polyethylene glycol molecular weight, 123,125/ High-performance liquid chromatography (HPLC) cucurbitacins Β and E, 108,109/, 204,205/ High-speed countercurrent chromatography separation of alkaloids from Senecio fuberi Hemsl, separation of cucurbitacin Β and Ε from fruit base of Cucumis melo L., separation of gardenia yellow component,

4 INDEX 235 High-speed countercurrent chromatography Continued on-line FAB MS detection through moving belt interface, Human immunodeficiency virus 1 (HTV-1) aspartyl proteinase substrate peptide, purification, design of assay, experimental procedure, product generation, solvent system, 116,118 tritiated peptide separation, 116,117/ Human serum, high- and low-density lipoprotein fraction isolated by Indole auxins, ph-zone-refining 174,177/ Interfacial area between phases in channels, definition, 70,72 Isolation, high- and low-density lipoprotein fractions from human serum by L Linear velocity, definition, 63 Lipophilicity conceptual analysis, 143,147/ relationship to biological activity, 143 structural information encoded, 149,151 Lipophilicity-derived structural parameters, application to quantitative structure-activity relationships, Lipoprotein fractions from human serum, isolation by countercurrent chromatography, Liquid flow, coil planet centrifuge chromatography, 5,7,8/ Liquid-liquid partition coefficients measurement techniques, 144 solute retention, 32,34 Liquid partition chromatography, limitations, 156 Liquid polarity and partition coefficient, and stationary-phase retention in indexes, 22-25/ selection parameters, 20,22-24 Low- and high-density lipoprotein fractions from human serum isolation by M Mathematical model of ph-zone-refining apparent partition coefficient of retainer acid at plateau, 164 elution rate of trailing border of retainer acid, multiple solute zones and mutual relationship, retention volume of retainer acid, solute zone formation behind sharp retainer border, Measurement, partition coefficient, using centrifugal partition chromatography, l-methyl-4-methoxymethylcyclohexanecarboxylic acid, ph-zone-refining 178,179/ Mobile phase in centrifugal partition chromatography, flow pattern model, Mobile-phase volume to column volume ratio, importance, 62 Model, flow pattern of mobile phase in centrifugal partition chromatography, Monoprotic acids mixture, ph-zone-refining 194,196/ plateau concentration, 197

5 236 MODERN COUNTERCURRENT CHROMATOGRAPHY Moving belt interface on-line FAB MS detection in high-speed schematic representation, 130,131/ Ν Neoplatyphylline, separation from Senecio fuberi Hemsl chromatography, Nonaqueous solvent systems, stationaryphase retention in countercurrent chromatography, 32,33/ Number of theoretical plates, Octanol-water system, partition coefficients, 149,151 On-line FAB MS detection in high-speed countercurrent chromatography through moving belt interface, advantages, 129 dipeptides, / erythromycins, 133, / experimental procedure, 130,132,135,137 schematic representation, 130,131/ Optimal settings, experimental design for determination for cross-axis coil planet centrifuge, Optimization of countercurrent chromatographic solvent systems, empirical partitioning in systems of varying polarity, approximate partition coefficients, initial need for semiquantitative monitoring system, 79 optimization, various systems, 80 tylophoroside isolation and purification, Orbital turns per theoretical plate for comparison of countercurrent chromatographic devices, apparatus, 38 count of orbital turns per plate, 44,45/ Orbital turns per theoretical plate for comparison of countercurrent chromatographic devices Continued effective linear velocity of mobile phase, 39,42/ efficiency, 39,43-44 experimental conditions, 38-40/ retention of stationary phase, 39,41/ solvent systems and solutes, 38 theory, Ρ Partition coefficient and sample recovery, 2-3 in heptane-water systems, 151 in octanol-water systems, 149,151 measurement using centrifugal partition chromatography, Period of motion of column around central axis of apparatus, definition, 37 ph of mobile phase in equilibrated solute zone, calculation, 167 chromatography advantages, 156,218 apparatus, 169 comparison to displacement chromatography, 178, D&C Orange No. 5, 174, / description, 10-12, development, 218 dinitrophenylamino acids, eluate analysis, 170,172 equilibrium model, indole auxins, 174,177/ mathematical model, methyl-4-methoxymethylcyclohexanecarboxylic acid, 178,179/ number of components, 157, preparative separation, principle, L-proline benzyl ester, 178,181/ reagents, 169 sample size, 157, separation procedure, 170

6 INDEX 237 ph-zone-refming countercurrent chromatography Continued solvent phases to initiate model experiments, 157,158/ component separation, two-phase solvent system and sample solution, 170,17 If Plates, theory, 35 Platyphylline, separation from Senecio fuberi Hemsl by high-speed Polarity of countercurrent chromatography solvents, definitions, 17 Preparative separation, components by ph-zonerefining L-Proline benzyl ester, ph-zonerefining countercurrent chromatography, 178,181/ Purification HTV-1 aspartyl proteinase substrate peptide, components by ph-zone-refining Q Quantitative structure-activity relationships, application of lipophilicity-derived structural parameters, R Raclopride, quantitative structureactivity relationships, 152/153 Resolution, countercurrent chromatography theory, 9-10 Response, chromatographic, definition, 49 Retainer acid or retaining acid chromatography, plateau ph prediction, 194, / Retainer acid orretainingacid Continued purification, 226,22'yf Retention percentage, definition, 20 Retention volume of retainer acid, calculation, Reverse transcriptase inhibitor drugs, examples, 111 S Sample acids, plateau ph prediction, 197,200 Sample recovery, determination, 2 Sample size, component purification, Senecio fuberi Hemsl, separation of alkaloids chromatography, Separation chromatography alkaloids from Senecio fuberi Hemsl, cucurbitacins Β and Ε from fruit base of Cucumis melo L., gardenia yellow components, Serum lipoproteins, chromatographic separations, 119 Solubility parameter, definition, 20,24 Solute properties, determination by measurement of partition coefficient, Solvent(s) composition, purification, 226, list, 24,26-27r polarity, influencing factors, 20 polarity indexes, 22-25/ selection parameters, 20,22-24 systems in countercurrent chromatography, 10 Squalidine, separation from Senecio fuberi Hemsl by high-speed Stationary-phase loss rate, definition, 20 Stationary-phase retention in 16-34

7 238 MODERN COUNTERCURRENT CHROMATOGRAPHY Stationary-phase retention Continued chromatographic system, experimental procedure, initial stationary-phase retention, 24,28-30 liquid-liquid partition coefficient, 32,34 nonaqueous solvent systems, 32,33/ rate of stationary-phase loss, 30,32 solvent polarity indexes, 22-25/ solvent selection parameters, 20,22-24 solvents used, 24,26-27* stable stationary-phase retention, 30,31/ theoretical model, 20,21/ Stationary-phase volume, definition, 18 Stokes' law, basis of flow pattern model of mobile phase in centrifugal partition chromatography, Structural determinants of solubility-related molecular properties of neutral organic solutes in solution, calculation, 149 Structural information, encoded in lipophilicity, 149,151 4,5,6,7-Tetrachlorofluorescein, HPLC analyses, 204,205/ synthesis, / 4,5,6,7-Tetrachlorofluorescein purification by ph-zone-refining apparatus, elution profile, experimental procedure, HPLC analyses of fractions, mobile-phase ammonia concentration, 226,227/ 4,5,6,7-Tetrachlorofluorescein Continued purification by ph-zone-refining countercurrent chromatography Continued retainer acid, 226, sample size, solvent composition, 226, separation by ph-zone-refining byproduct formation, 211,215/ characterization of compounds, 211, / chromatograms, 209,210/ compounds isolated, 209,211,212/ condensation of tetrachlorophthalic anhydride with resorcinol molecules, 211,212/ experimental procedure, sample size, 211, / Theoretical plates, description, 35 Theory of plates, development, 35 Tylophoroside, isolation and purification by empirical partitioning, 81 final purification, initial isolation, 84 semiquantitative monitor development, 81,83/ structures, 81,82/ Type J coil planet centrifuges, comparison using orbital turns per theoretical plate, Versatility, countercurrent chromatography, 3