{"title":"Preparative Liquid Chromatography and the H/u Curve*","authors":"C. Dewaele, M. De Coninck, M. Verzele","doi":"10.1201/9781003210108-7","DOIUrl":"https://doi.org/10.1201/9781003210108-7","url":null,"abstract":"","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"45 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2021-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"131750004","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2021-07-29DOI: 10.1201/9781003210108-15
E. Soczewiński, K. Czapinska, Teresa Wawryznowicz
{"title":"Migration of Zones of Test Dyes in Preparative Thin-Layer Chromatography: Stepwise Gradient Elution","authors":"E. Soczewiński, K. Czapinska, Teresa Wawryznowicz","doi":"10.1201/9781003210108-15","DOIUrl":"https://doi.org/10.1201/9781003210108-15","url":null,"abstract":"","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"06 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2021-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"128916691","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057624
Y. Ito
Abstract Potential capability of the apparatus in performing countercurrent chroma-tography has been examined with three different types of coiled columns, all coaxially mounted around the holder. In single-layer coils, typical solvent systems display characteristic hydrodynamic distribution which ensures a stable retention of the stationary phase against heavy sample loading in preparative separations. Direct observation of the hydrodynamic motion in the rotating spiral column revealed vigorous mixing of the two solvent phases throughout the area which promises a high partition efficiency of the present method. Gram-quantity preparative separations were performed in the multilayer coil with two different sets of test samples: Isocratic elution of dinitrophenyl amino acids yielded high partition efficiency of 1600 theoretical plates while the versatility of the method was demonstrated on gradient elution of dipeptides including two pairs of sequential isomers.
{"title":"Cross-Axis Synchronous Flow-Through Coil Planet Centrifuge Free of Rotary Seals for Preparative Countercurrent Chromatography. Part II. Studies on Phase Distribution and Partition Efficiency in Coaxial Coils","authors":"Y. Ito","doi":"10.1080/01496398708057624","DOIUrl":"https://doi.org/10.1080/01496398708057624","url":null,"abstract":"Abstract Potential capability of the apparatus in performing countercurrent chroma-tography has been examined with three different types of coiled columns, all coaxially mounted around the holder. In single-layer coils, typical solvent systems display characteristic hydrodynamic distribution which ensures a stable retention of the stationary phase against heavy sample loading in preparative separations. Direct observation of the hydrodynamic motion in the rotating spiral column revealed vigorous mixing of the two solvent phases throughout the area which promises a high partition efficiency of the present method. Gram-quantity preparative separations were performed in the multilayer coil with two different sets of test samples: Isocratic elution of dinitrophenyl amino acids yielded high partition efficiency of 1600 theoretical plates while the versatility of the method was demonstrated on gradient elution of dipeptides including two pairs of sequential isomers.","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"36 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"122736374","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057615
D. Wilson
Abstract The effects of solute-solute interactions on the shapes of the bands in preparative gas chromatography are modeled by numerical integration of the coupled sets of differential equations describing solute movement An asymmetrical upwind algorithm is used to describe advection; this greatly reduces the numerical dispersion which is inherent in the theoretical plate method. A microcomputer was used for doing the computations.
{"title":"Line Shapes in Gas Chromatography. III. Solute-Solute Interactions in Preparative Columns","authors":"D. Wilson","doi":"10.1080/01496398708057615","DOIUrl":"https://doi.org/10.1080/01496398708057615","url":null,"abstract":"Abstract The effects of solute-solute interactions on the shapes of the bands in preparative gas chromatography are modeled by numerical integration of the coupled sets of differential equations describing solute movement An asymmetrical upwind algorithm is used to describe advection; this greatly reduces the numerical dispersion which is inherent in the theoretical plate method. A microcomputer was used for doing the computations.","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"43 2 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"121690364","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057627
H. Schott
Abstract DNA is chemically degraded to a mixture of pure oligonucleotides. From the resulting partial hydrolyzate, defined oligonucleotides with two to six monomer units and defined mixtures of sequence-isomeric purine oligonucleotides are isolated in preparative amounts. The partial hydrolyzate is fractionated by a chromatographic separation route which uses anion-exchange chromatography on DEAE- and QAE-Sephadex at different pH values, paper chromatography, and reversed-phase HPLC. The sequence of the isolated oligonucleotides and the composition of the mixtures of sequence-isomers were determined from chromatographic data, absorption characteristics, enzymatic degradation, and “fingerprints.”
{"title":"Preparative Isolation of Purine Oligonucleotides from Partial Hydrolyzates of Depyrimidinated DNA","authors":"H. Schott","doi":"10.1080/01496398708057627","DOIUrl":"https://doi.org/10.1080/01496398708057627","url":null,"abstract":"Abstract DNA is chemically degraded to a mixture of pure oligonucleotides. From the resulting partial hydrolyzate, defined oligonucleotides with two to six monomer units and defined mixtures of sequence-isomeric purine oligonucleotides are isolated in preparative amounts. The partial hydrolyzate is fractionated by a chromatographic separation route which uses anion-exchange chromatography on DEAE- and QAE-Sephadex at different pH values, paper chromatography, and reversed-phase HPLC. The sequence of the isolated oligonucleotides and the composition of the mixtures of sequence-isomers were determined from chromatographic data, absorption characteristics, enzymatic degradation, and “fingerprints.”","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"18 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"122181056","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057622
P. Gareil, R. Rosset
Abstract The shape of nonlinear elution peaks was studied experimentally in various chromatographic modes and a wide sample size range encompassing the case where the distribution isotherm curvature is the prevailing factor of band broadening. It is shown that as sample size is varied, the tailing part of all peaks adjoins a common curve that can be fitted with an exponential function whose parameters are independent of mobile phase linear velocity and stationary phase particle size. The effect of solute capacity factor on these parameters was also investigated. These findings provide valuable help for the optimization of linear velocity, particle size, as well as sample size in preparative liquid chromatography under mass overload conditions.
{"title":"Experimental Characterization of Strongly Nonlinear Elution Peaks in Liquid Chromatography","authors":"P. Gareil, R. Rosset","doi":"10.1080/01496398708057622","DOIUrl":"https://doi.org/10.1080/01496398708057622","url":null,"abstract":"Abstract The shape of nonlinear elution peaks was studied experimentally in various chromatographic modes and a wide sample size range encompassing the case where the distribution isotherm curvature is the prevailing factor of band broadening. It is shown that as sample size is varied, the tailing part of all peaks adjoins a common curve that can be fitted with an exponential function whose parameters are independent of mobile phase linear velocity and stationary phase particle size. The effect of solute capacity factor on these parameters was also investigated. These findings provide valuable help for the optimization of linear velocity, particle size, as well as sample size in preparative liquid chromatography under mass overload conditions.","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"1 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"130339888","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057618
G. Crétier, J. Rocca
Abstract This paper describes the effect of injection volume on injectable sample load consistent with purity and recovery ratio of the solute of interest for different shapes of solute isotherms (convex or concave, without or with interactions between two adjacent solute bands). In preparative liquid chromatography, the column mass overloading conditions are usually thought to be better than volume overload conditions; according to this study, this statement is shown not to be true in all cases because optimization of injection conditions is much more complicated. For some isotherm shapes, there is an optimal injection volume in which injectable sample load is maximum.
{"title":"Optimization of Injection Conditions in Preparative Liquid Chromatography","authors":"G. Crétier, J. Rocca","doi":"10.1080/01496398708057618","DOIUrl":"https://doi.org/10.1080/01496398708057618","url":null,"abstract":"Abstract This paper describes the effect of injection volume on injectable sample load consistent with purity and recovery ratio of the solute of interest for different shapes of solute isotherms (convex or concave, without or with interactions between two adjacent solute bands). In preparative liquid chromatography, the column mass overloading conditions are usually thought to be better than volume overload conditions; according to this study, this statement is shown not to be true in all cases because optimization of injection conditions is much more complicated. For some isotherm shapes, there is an optimal injection volume in which injectable sample load is maximum.","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"8 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"127973467","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057617
K. Hupe, B. Hoffmann
Abstract The amount of substance that can be separated per unit of time (the production rate) and the purity of the isolated compounds are the determining quantities in preparative chromatography. The production rate in combination with a certain resolution (i.e., a certain selectivity and a certain number of theoretical plates) are therefore the overruling optimization criteria for the design and operation of a preparative chromatographic system.
{"title":"Optimum Conditions in Preparative Liquid Chromatography. II. Selection of Column Dimensions","authors":"K. Hupe, B. Hoffmann","doi":"10.1080/01496398708057617","DOIUrl":"https://doi.org/10.1080/01496398708057617","url":null,"abstract":"Abstract The amount of substance that can be separated per unit of time (the production rate) and the purity of the isolated compounds are the determining quantities in preparative chromatography. The production rate in combination with a certain resolution (i.e., a certain selectivity and a certain number of theoretical plates) are therefore the overruling optimization criteria for the design and operation of a preparative chromatographic system.","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"20 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"130213459","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057619
V. R. Meyer
Abstract The H/u curves of two HPLC columns of 10 mm i.d., filled with silica of a particle diameter of 5 and 25–40 μm, respectively, have been determined at various amounts of injected sample. Indications of mass overload, Le, peak broadening, occur at a sample load of 10 μg/g for the column with 5 μm silica but not until 100 μg/g for the column with coarse stationary phase. Although H values increase markedly with higher sample mass, the slopes of the H/u curves remain almost constant on both columns up to samples of 1 mg/g. This means the relative increase of the plate height with increasing flow velocity becomes nearly negligible under conditions of moderate mass overload. However, by increasing the sample load up to 5 or 10 mg/g, the H/u curves show a dramatic increase of slope: at high mass overload the mobile phase flow rate cannot be increased without a remarkable decrease in column performance.
{"title":"The Influence of Sample Mass and Flow Velocity on Performance in Preparative Column Liquid Chromatography","authors":"V. R. Meyer","doi":"10.1080/01496398708057619","DOIUrl":"https://doi.org/10.1080/01496398708057619","url":null,"abstract":"Abstract The H/u curves of two HPLC columns of 10 mm i.d., filled with silica of a particle diameter of 5 and 25–40 μm, respectively, have been determined at various amounts of injected sample. Indications of mass overload, Le, peak broadening, occur at a sample load of 10 μg/g for the column with 5 μm silica but not until 100 μg/g for the column with coarse stationary phase. Although H values increase markedly with higher sample mass, the slopes of the H/u curves remain almost constant on both columns up to samples of 1 mg/g. This means the relative increase of the plate height with increasing flow velocity becomes nearly negligible under conditions of moderate mass overload. However, by increasing the sample load up to 5 or 10 mg/g, the H/u curves show a dramatic increase of slope: at high mass overload the mobile phase flow rate cannot be increased without a remarkable decrease in column performance.","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"35 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"127008973","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1987-08-01DOI: 10.1080/01496398708057626
G. Leaver, J. Conder, J. Howell
Abstract The conditions of operation of ion-exchange Chromatography are examined for the production of albumin from bovine serum and plasma. The ion-exchanger is a Vistec-DEAE cellulose. Of the various modes of chromatographic operation available, the most suitable for proteins is shown to be adsorption onto the whole column followed by stepwise elution. The method is developed by studying; experimentally, the effect of major parameters so as to point the way to optimization. Prior dialysis and dilution of the feed are beneficial. Other conclusions apply to the large-scale separation of proteins in general. In particular, column length, eluent velocity, feed band width, and packing rigidity are parameters where trade-offs will be needed to maximize performance. If suitable precautions are taken in column design, scale-up can be achieved by increasing the column diameter alone. Albumin separated chromatographically is superior in electrophoretic purity to that produced by the commercial Cohn precipitation ...
{"title":"A Method Development Study of the Production of Albumin from Animal Blood by Ion-Exchange Chromatography","authors":"G. Leaver, J. Conder, J. Howell","doi":"10.1080/01496398708057626","DOIUrl":"https://doi.org/10.1080/01496398708057626","url":null,"abstract":"Abstract The conditions of operation of ion-exchange Chromatography are examined for the production of albumin from bovine serum and plasma. The ion-exchanger is a Vistec-DEAE cellulose. Of the various modes of chromatographic operation available, the most suitable for proteins is shown to be adsorption onto the whole column followed by stepwise elution. The method is developed by studying; experimentally, the effect of major parameters so as to point the way to optimization. Prior dialysis and dilution of the feed are beneficial. Other conclusions apply to the large-scale separation of proteins in general. In particular, column length, eluent velocity, feed band width, and packing rigidity are parameters where trade-offs will be needed to maximize performance. If suitable precautions are taken in column design, scale-up can be achieved by increasing the column diameter alone. Albumin separated chromatographically is superior in electrophoretic purity to that produced by the commercial Cohn precipitation ...","PeriodicalId":184327,"journal":{"name":"Preparative-Scale Chromatography","volume":"14 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"1987-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"127804298","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：