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A cation-exchange material for protein separations based on grafting of thiol-terminated sulfopropyl methacrylate telomers onto hydrophilized monodisperse divinylbenzene particles
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
2008 (English)In: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 31, no 12, 2143-2150 p.Article in journal (Refereed) Published
Abstract [en]

A strong cation-exchange separation material has been prepared from monodisperse divinylbenzene particles modified by a grafting to approach, utilizing as anchoring points epoxy groups introduced onto the surface of the particles via oxidation of residual vinyl groups. The grafted chains consisted of thiol-terminated telomers of sulfopropyl methacrylate prepared by iniferter mediated polymerization, and grafting was performed by reaction of the corresponding thiolate anion with the surface epoxy groups. Attachment through epoxy moieties that were subsequently converted into 2,3-propanediol groups increased the hydrophilicity of the polymeric particles and incubation experiments showed no signs of the proteins denaturing on the column during an extended contact time of 1 h at room temperature. The performance of the grafted material was demonstrated by the chromatographic separation of cytochrome C, lysozyme, myoglobin, and ribonuclease A, in a cation-exchange mode.

Place, publisher, year, edition, pages
2008. Vol. 31, no 12, 2143-2150 p.
Keyword [en]
Grafting to, Photoinitiation, Polymeric particles, Protein separation, Precipitation polymerization
Identifiers
URN: urn:nbn:se:umu:diva-10270DOI: doi:10.1002/jssc.200800180PubMedID: 18615833OAI: oai:DiVA.org:umu-10270DiVA: diva2:149941
Available from: 2008-08-06 Created: 2008-08-06 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Synthesis and modifications of materials for separation science
Open this publication in new window or tab >>Synthesis and modifications of materials for separation science
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis deals with the preparation of materials for use in separation science and their surface modification by grafting. The overall aim is the preparation of diverse materials by combination of a set of developed tools.

Included in the thesis is the synthesis of monolithic media using non-traditional crosslinkers, the characterization of their porous properties and initial testing in reversed-phase chromatographic separation of proteins. The preparation of a library of short polymer chains, telomers, with varied functionality and their characterization is reported. Included in the characterization is the gradient polymer elution chromatography of selected telomers on a monolithic column in capillary format. The technique shows promise as a tool for monitoring of polymerization processes and for the separation of telomers with similar size but different functionalities or characteristics.

Finally, the combination of polymeric support materials and the prepared telomer library is used in surface modification. Surface modification is performed onto activated surfaces via a “grafting to” approach. One example is shown, the surface modification of epoxy-modified divinylbenzene particles by attachment of telomer chains introducing ion-exchange functionality. The material is tested for the separation of proteins, in ion-exchange chromatography mode.

Place, publisher, year, edition, pages
Umeå: Kemi, 2008. 43 p.
Keyword
material synthesis, monolith, surface modification, telomer, “grafting to”, gradient polymer elution, chromatography
National Category
Other Basic Medicine
Identifiers
urn:nbn:se:umu:diva-1572 (URN)978-91-7264-528-8 (ISBN)
Public defence
2008-03-28, N360, Naturvetarhuset, Umeå Universitet, Umeå, 10:00 (English)
Opponent
Supervisors
Available from: 2008-03-07 Created: 2008-03-07 Last updated: 2017-05-18Bibliographically approved
2. Synthesis and modification of monodisperse polymer particles for chromatography
Open this publication in new window or tab >>Synthesis and modification of monodisperse polymer particles for chromatography
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Liquid chromatography is an analytical technique that is constantly facing new challenges in the separation of small molecules and large biomacromolecules. Recently the development of ultra high pressure liquid chromatography has increased the demand on sturdy particles as stationary phase. At the same time the particle size has decreased to sub-2 µm and packed into shorter analytical columns. This thesis deals with the development of new ways of preparing particulate polymer materials using divinylbenzene (DVB) as crosslinker. It includes a novel procedure for synthesizing monodisperse polymer particles by photoinitiated precipitation polymerization. A 150 W short arc xenon lamp was used to initiate the polymerizations. The synthesized particles are monodisperse and have an average particle size ranging from 1.5 to 4 μm depending on reaction conditions and have subsequently been used as grafting templates. The surface of DVB particles contains residual vinyl groups that serve as anchoring points for further functionalization via a variety of grafting schemes. Copolymerization with incorporation of 2,3-epoxypropyl methacrylate yielded pendant oxirane groups on the particle surface. Atom transfer radical polymerization (ATRP) was used to graft methacrylates from the surface resulting in a core-shell type material. A “grafting to” scheme was used to attach pre-made sulfopropyl methacrylate telomers onto particles containing oxirane rings.

Abstract [sv]

Populärvetenskaplig sammanfattning på svenska:

Vätskekromatografi är en analytisk kemisk teknik som ständigt står inför nya utmaningar när det gäller att separera allt från små organiska föreningar till stora makro¬molekyler. Denna avhandling beskriver tillverkning av polymera partiklar med exceptionellt jämn storleksfördelning och ytmodifiering av dessa, för användning som stationärfas i kromatografi¬kolonner. Polymeriserings¬tekniken som används är utfällnings¬polymerisering där lösningen UV-bestrålas av en 150 W xenonlampa. Monomeren (byggstenen) löses tillsammans med en intiator i ett lösningsmedel och efterhand som polymeriseringen fortskrider faller polymerpartiklarna ut. Polymerpartiklarna är gjorda av monomeren divinylbensen som fungerar som en tvärbindare, dvs att den länkar ihop flera kedjor till ett hårt litet nystan. Partiklarna växte till en storlek på 1,5 till 4 µm under två till fyra dygn.

Efter tillverkningen är partiklarnas yta täckta av vinylgrupper som kan användas för att fästa funktionella polymerkedjor. Genom att tillföra monomeren 2,3-epoxipropyl¬metakrylat i polymeriseringen kunde man desutom få en partikelyta som innehöll epoxigrupper. Epoxigrupperna användes för att fästa positivt laddade polymerkedjor av bestämd längd. Materialet packades i en kromatografikolonn och användes för att separera en testlösning bestående av fyra proteiner.

Partiklarna användes även som bas för ymppolymerisering där den vinyltäckta ytan fått reagera med vätebromid. Detta gör att partiklarna blir stora makroinitiatorer som kan användas för att på ett kontrollerat sätt låta polymerkedjor växa från ytan. I en undersökning ympades 2,3-epoxypropylmetakrylat från ytan på partiklarna och resultatet blev ett tjockt ytskikt. Epoxigrupperna kunde sedan hydrolyseras till dioler vilket gjorde partiklarna mer hydrofila.

Place, publisher, year, edition, pages
Umeå: Kemi, 2008. 45 p.
Keyword
Polymer particles; photoinitiation; precipitation polymerization; styrene; divinylbenzene; atom transfer radical polymerization; liquid chromatography
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:umu:diva-1948 (URN)978-91-7264-709-1 (ISBN)
Public defence
2009-01-23, KB3A9, KBC-huset, Linneaus väg, Umeå Universitet, Umeå, 10:00 (English)
Opponent
Supervisors
Available from: 2008-12-18 Created: 2008-12-18 Last updated: 2009-11-20Bibliographically approved

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