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Theoretical and experimental study of binary perturbation peaks with focus on peculiar retention behaviour and vanishing peaks in chiral liquid chromatography
Uppsala University, Disciplinary Domain of Science and Technology, Mathematics and Computer Science, Department of Information Technology, Division of Scientific Computing. Uppsala University, Disciplinary Domain of Science and Technology, Mathematics and Computer Science, Department of Information Technology, Numerical Analysis.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Surface Biotechnology.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Surface Biotechnology.
2003 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 991, 31-45 p.Article in journal (Refereed) Published
Place, publisher, year, edition, pages
2003. Vol. 991, 31-45 p.
Keyword [en]
perturbation method, adsorption isotherms, enantiomer separation, retention behaviour
National Category
Analytical Chemistry Computational Mathematics
Identifiers
URN: urn:nbn:se:uu:diva-91957DOI: 10.1016/S0021-9673(03)00213-9OAI: oai:DiVA.org:uu-91957DiVA: diva2:164874
Available from: 2004-09-01 Created: 2004-09-01 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Development and Validation of HPLC Methods for Analytical and Preparative Purposes
Open this publication in new window or tab >>Development and Validation of HPLC Methods for Analytical and Preparative Purposes
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis concerns the development and validation of high performance liquid chromatography (HPLC) methods aimed for two industrially important areas: (i) analysis of biotechnological synthesis and (ii) determination of adsorption isotherm parameters. There is today a lack of detailed recommendations for analytical procedures in the field of biotechnological production of drugs. Therefore, guidelines were given for analytical development and validation in this field; the production of 9α-hydroxyprogesterone was used as model. In addition, a rapid method using HPLC coupled with diode-array-detection (DAD) and mass spectrometry (MS), was developed for the preliminary identification and quantification of the product. In addition, requirements and recommendations were developed for the selection of the internal standard and for its inclusion in the process liquid. By using this approach the precision and accuracy of the quantitative method were considerably improved.

Preparative chromatography is a powerful separation method for the purification of pure compounds from more or less complex sample mixtures. One such mixture can be the process liquid from a fermentation, another example can be a racemic mixture of compounds whose enantiomeric constituents must be isolated. Computer-assisted modeling can be used to optimize preparative chromatography. However, competitive adsorption isotherm parameters are required as input data for the computer simulations. In this thesis, a new injection technique, based on a firm theoretical basis, was developed for the peak perturbation (PP) method allowing the determination of binary competitive adsorption isotherm parameters from a broad concentration range. With the new method the determination of adsorption isotherm parameters from a quaternary mixture could be done for the first time. The profiles simulated with these parameters showed excellent agreement with the corresponding experimental profiles, validating the accuracy of the adsorption isotherm parameters derived by the new method.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2004. 87 p.
Series
Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1104-232X ; 995
Keyword
Chemistry, High performance liquid chromatography (HPLC), Analytical biotechnology, Sample preparation, Diode-array-detection (DAD), Mass spectrometry (MS), Validation, Preparative chromatography, Competitive isotherm parameters, Perturbation peak (PP) method, Kemi
National Category
Chemical Sciences
Identifiers
urn:nbn:se:uu:diva-4442 (URN)91-554-6005-4 (ISBN)
Public defence
2004-09-24, Room B42, BMC, Husargatan 3, Uppsala, 13:15
Opponent
Supervisors
Available from: 2004-09-01 Created: 2004-09-01Bibliographically approved
2. Adsorption Isotherm Parameter Estimation in Nonlinear Liquid Chromatography
Open this publication in new window or tab >>Adsorption Isotherm Parameter Estimation in Nonlinear Liquid Chromatography
2005 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis concerns the development and validation of methods for the industrially important area of adsorption isotherm parameter estimation in preparative, nonlinear high performance liquid chromatography (HPLC). Preparative chromatography is a powerful separation method to get pure compounds from more or less complex liquid mixtures, e.g., mixtures of mirror-image molecules. Computer simulations can be used to optimize preparative chromatography, but then competitive adsorption isotherm parameters are usually required. Here two methods to estimate adsorption isotherm parameters are treated: (i) the perturbation peak (PP) method and (ii) the inverse method (IM).

A new theory for the PP method was derived and led to a new injection technique which was validated experimentally. This injection technique solved the severe problem with vanishing peaks and enabled us to use the PP method to estimate binary competitive adsorption isotherms valid over a broad concentration range. Also, the injection technique made it possible to estimate competitive adsorption isotherms for a quaternary mixture for the first time. Finally, an interesting perturbation peak phenomenon, known as the “Helfferich Paradox”, was experimentally verified for the first time.

The IM is a relatively new method to determine adsorption isotherm parameters. It has the advantage of requiring very small samples, but also requires an advanced computer algorithm. An improved implementation of this computer algorithm was developed and tested experimentally. Also, a variant of the IM called “the inverse method on plateaus” was tested experimentally and the estimated adsorption isotherm parameters were shown to be valid over a broader concentration range than those estimated with the standard IM.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2005. 24 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 96
Keyword
High performance liquid chromatography (HPLC), Preparative chromatography, Competitive adsorption isotherm parameters, Perturbation peak (PP) method, Inverse method (IM), Computer simulation, Parameter estimation, Numerical method
National Category
Computational Mathematics Analytical Chemistry
Research subject
Scientific Computing
Identifiers
urn:nbn:se:uu:diva-5971 (URN)91-554-6355-X (ISBN)
Public defence
2005-10-19, Room B21, Uppsala Biomedical Centre, Husargatan 3, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2005-09-27 Created: 2005-09-27 Last updated: 2011-10-27Bibliographically approved

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