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Thesis “Fundamental Investigations of Adsorption in SFC”

On the 20th of March 2020 Emelie Glenne will defend her thesis on Supercritical Fluid Chromatography titled “Fundamental Investigations of Adsorption in SFC”

Where: Nyquistsalen, 9C 203, Karlstads universitet, Karlstad
When: 20/3 at 10:00

Download thesis here

Download papers:

Paper I : A closer study of methanol adsorption and its impact on solute retentions in supercritical fluid chromatography

Paper II:Peak deformations in preparative supercritical fluid chromatography due to co-solvent adsorption

Paper III: Systematic investigations of peak deformations due to co-solvent adsorption in preparative supercritical fluid chromatography

ABSTRACT

In supercritical fluid chromatography (SFC) the mobile phase is composed by carbon dioxide as the main weak solvent, in a condition between a gas and a liquid. The interest in SFC has recently increased due to several advantages compared to traditional liquid chromatography (LC) such as faster sample throughput and lower environmental impact. However, there is still a lack of fundamental knowledge about SFC, among others, due to the compressible mobile phase. This thesis work aims at a deeper understanding of the functions of the mobile phase components used in SFC through systematic adsorption studies. 

In Paper I, surface excess adsorption isotherms of the co-solvent methanol on a diol silica adsorbent was investigated. It was revealed that a monolayer of methanol was formed. In Paper II, severe peak deformation effects due to this adsorption were revealed, and it was demonstrated under which conditions these deformations appear and how the co-solvent fraction can tune the shape of the eluted peak. The findings in these papers revealed that a competitive additive model best predicts the solute retention at low methanol fractions whereas at higher fractions, when a solvent layer has formed, methanol acts just as a modifier. In Paper III, the generality of the effects was proven by investigations of other co-solvent/stationary phase combinations. In Paper IV it was investigated how the robustness of SFC separations depend on the co-solvent adsorption, pressure, and temperature. In Paper V, the impact of the addition of amine additives on separation performance was investigated. Two different underlying mechanisms for solute peak distortions were revealed: (i) deformations generated by the perturbation peak and (ii) deformation due to multilayer formation promoted by the additive.

The deeper knowledge about SFC obtained in this thesis provides guidelines for development of more robust SFC methods for analysis and preparative separations where peak distortions can be avoided.

SFC 2019 Philadelphia

We gave one lectures and presented two posters at the SFC 2019 conference in Philadelphia .

Lectures

  1. A New Strategy for Improved Method Transfer and Scale-Up in SFC Martin Enmark, Marek Szymanski, Jörgen Samuelsson and Torgny Fornstedt

Posters

  1. A New Strategy for Improved Method Transfer and Scale Up in SFC Martin Enmark, Marek Szymanski, Jörgen Samuelsson and Torgny Fornstedt
  2. Peak Distortions in SFC Due to the Mobile Phase Composition Martin Enmark, Emelie Glenne, Marek Lesko, Fredrik Limé, Jörgen Samuelson and Torgny Fornstedt

For more information please visit the symposium web-page https://www.greenchemistrygroup.org/scientific-program/sfc-2019

PREP 2019 Baltimore

We gave two lectures and presented three posters at the 32nd International Symposium on Preparative and Process Chromatography in Baltimore 2019.

Lectures

1.Preparative Separation of Phosphorothioated Antisense Oligonucleotides. Martin Enmark, Joakim Bagge, Jörgen Samuelsson, LindaThunberg, Hanna Leek, Fredrik Lime, Per Jageland, Torgny Fornstedt.

2.Preparative Supercritical Fluid Chromatography Separation of Peptides:On the Issue of Solubility and Robustness. Joakim Bagge, Martin Enmark, Marek Lesko, Emelie Glenne,Linda Thunberg, Annika Langborg Weinmann, Tomas Leek, Hanna Leek, Fredrik Limé,Jörgen Samuelsson, Torgny Fornstedt. 

For more information please visit the symposium web-page http://prepsymposium.org/index.html

HPLC 2019 Milan

We gave two lectures and presented three posters at the 48th International Symposium on High Performance Liquid Phase Separations and Related Techniques in Milan, Italy 2019.

Lectures

1. (Invited lecture) Modern Supercritical Fluid Chromatography – Impact of Mobile Phase Composition T. Fornstedt, E. Glenne, M. Enmark, M. Lésko, F. Limé, J.Samuelsson.

2. Purification of Phosphorothioated Antisense Oligonucleotides. M. Enmark, J.Bagge, J. Samuelsson, L. Thunberg, H. Leek, F. Limé, T. Fornstedt.

For more information please visit https://www.hplc2019-milan.org/

HPLC 2018 Washington

We gave a lecture and presented three posters at the 47th International Symposium on High Performance Liquid Phase Separations and Related Techniques in Washington D.C. 2018.

 

 

 

 

Lecture:
“On the Issue of Separating Diastereomers of Phosphorothioated
Oligonucleotides.”		 Torgny Fornstedt(1), Martin Enmark(1), Jörgen Samuelsson(1), Maria Rova(1), Eivor Örnskov(2), Anders Karlsson(2)

1. Karlstad University, Karlstad, SWEDEN;
2. AstraZeneca, Molndal, SWEDEN
Poster:
“Highlighting often Neglected Experimental Parameters in Analytical Supercritical
Fluid Chromatography.”		 Prof. Torgny Fornstedt(1) , Martin Enmark(1) ,  Jörgen Samuelsson(1), Anders Karsslon(2)

1. Karlstad University, Karlstad, SWEDEN;
2. AstraZeneca, Molndal, SWEDEN 
Poster:
“Why Gradient Elution Lead to Increased Robustness of SFC Separations.”		 Prof. Torgny Fornstedt(1), Martin Enmark(1) , Emelie Glenne(1) , Marek Lesko(1,2) , Annika Weinmann(3) , Tomas Leek(3) , Krzysztof Kaczmarski(2) , Magnus Klarqvist(3) , Jörgen Samuelsson(1)

1. Karlstad University, Karlstad, SWEDEN;
2. Rzeszow University of Technology, Rzeszow, POLAND;
3. AstraZeneca, Molndal, SWEDEN
 Poster:
“Diastereomer Separation of Phosphorothioated Oligonucleotides.”		 Prof. Torgny Fornstedt(1), Martin Enmark(1) , Jörgen Samuelsson(1), Maria Rova(1), Eivor Örnskov(2), Anders Karlsson(2)

1. Karlstad University, Karlstad, SWEDEN;
2. AstraZeneca, Molndal, SWEDEN

For more information please visit the symposium webpage:

http://www.hplc2018.org/

PREP 2018 Baltimore

We gave a keynote lecture and presented three posters at the 31st International Symposium on Preparative and Process Chromatography in Baltimore 2018.

 

 

 

 

Lecture:
“Increasing the Robustness of SFC: Examples from Chiral and Peptide Separations”		 Prof. Torgny Fornstedt(1) , Martin Enmark(1) , Emelie Glenne(1) , Marek Lesko(1,2) , Annika Weinmann(3) , Tomas Leek(3) , Krzysztof Kaczmarski(2) , Magnus Klarqvist(3) , Jörgen Samuelsson(1)

1. Karlstad University, Karlstad, SWEDEN;
2. Rzeszow University of Technology, Rzeszow, POLAND;
3. AstraZeneca, Molndal, SWEDEN 
Poster:
“Proper Operational Conditions in Supercritical Fluid Chromatography of Complex Molecules, Set vs. Real Conditions”		 Prof. Torgny Fornstedt(1) , Martin Enmark(1) ,  Jörgen Samuelsson(1), Anders Karsslon(2)

1. Karlstad University, Karlstad, SWEDEN;
2. AstraZeneca, Molndal, SWEDEN 
Poster:
“Robust Operation of SFC using Peptide and Chiral Model Systems.”		 Prof. Torgny Fornstedt(1) , Martin Enmark(1) , Emelie Glenne(1) , Marek Lesko(1,2) , Annika Weinmann(3) , Tomas Leek(3) , Krzysztof Kaczmarski(2) , Magnus Klarqvist(3) , Jörgen Samuelsson(1)

1. Karlstad University, Karlstad, SWEDEN;
2. Rzeszow University of Technology, Rzeszow, POLAND;
3. AstraZeneca, Molndal, SWEDEN
 Poster:
“Separation of Phosphorothioated Oligonucleotides and their Diastereomers”		 Prof. Torgny Fornstedt(1) , Martin Enmark(1) , Jörgen Samuelsson(1), Maria Rova(1), Eivor Örnskov(2), Anders Karlsson(2)

1. Karlstad University, Karlstad, SWEDEN;
2. AstraZeneca, Molndal, SWEDEN

For more information please visit the symposium webpage:

http://prepsymposium.org/index.html

Kick-Off Meeting for the KK-Synergy Project “Quality Control and Purification for New Biological Drugs”

Kick-Off Meeting for the KK-Synergy Project “Quality Control and Purification for New Biological Drugs”

On the 30th of November 2017 our research group, together with researchers from several companies and universities, had a most successful kick-off day at Karlstad University for our new KK-Synergy project. The aim of this project is to develop state-of-the-art quality control methods for biological pharmaceuticals, i.e., proteins or similar molecules, which mimics molecules in the body and are injected in the body to stimulate the immune system.

The project has a budget of approximately €2 million and four companies and three academic institutions participate: Attana AB, AstraZeneca, Akzo Nobel Pulp and Performance Chemicals AB, Ridgeview Instruments AB, Karlstad University, Linné University and Örebro University.

The picture below shows the kick-off day participants.

KK-kickoff-Kemivärlden-2017

An article (in Swedish) about the project can be found in ”Kemivärlden Biotech med Kemisk Tidskrift” number 8, December 2017 on page 8 (see link)

For additional information see also:

http://news.cision.com/attana/r/quality-control-of-biological-pharmaceuticals,c2411154

Kemivärlden nr 3 2017 p15-17