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Utilizing RAFT polymerization for the preparation of well-defined bicontinuous porous polymeric supports: application to liquid chromatography separation of biomolecules

Khodabandeh, A, Arrua, RD, Thickett, SC ORCID: 0000-0002-8168-3856 and Hilder, EF 2021 , 'Utilizing RAFT polymerization for the preparation of well-defined bicontinuous porous polymeric supports: application to liquid chromatography separation of biomolecules' , ACS Applied Materials and Interfaces, vol. 13, no. 27 , pp. 32075-32083 , doi: 10.1021/acsami.1c03542.

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Polymer-based monolithic high-performance liquid chromatography (HPLC) columns are normally obtained by conventional free-radical polymerization. Despite being straightforward, this approach has serious limitations with respect to controlling the structural homogeneity of the monolith. Herein, we explore a reversible additionfragmentation chain transfer (RAFT) polymerization method for the fabrication of porous polymers with well-defined porous morphology and surface chemistry in a confined 200 μm internal diameter (ID) capillary format. This is achieved via the controlled polymerization-induced phase separation (controlled PIPS) synthesis of poly(styrene-co-divinylbenzene) in the presence of a RAFT agent dissolved in an organic solvent. The effects of the radical initiator/RAFT molar ratio as well as the nature and amount of the organic solvent were studied to target cross-linked porous polymers that were chemically bonded to the inner wall of a modified silica-fused capillary. The morphological and surface properties of the obtained polymers were thoroughly characterized by in situ nuclear magnetic resonance (NMR) experiments, nitrogen adsorptiondesorption experiments, elemental analyses, field-emission scanning electron microscopy (FESEM), scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS) as well as time-of-flight secondary ion mass spectrometry (ToF-SIMS) revealing the physicochemical properties of these styrene-based materials. When compared with conventional synthetic methods, the controlled-PIPS approach affects the kinetics of polymerization by delaying the onset of phase separation, enabling the construction of materials with a smaller pore size. The results demonstrated the potential of the controlled-PIPS approach for the design of porous monolithic columns suitable for liquid separation of biomolecules such as peptides and proteins.

Item Type: Article
Authors/Creators:Khodabandeh, A and Arrua, RD and Thickett, SC and Hilder, EF
Keywords: porous monoliths, cross-linked polymers, phase-separation, separation science, RAFT polymerization
Journal or Publication Title: ACS Applied Materials and Interfaces
Publisher: American Chemical Society
ISSN: 1944-8244
DOI / ID Number: 10.1021/acsami.1c03542
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© 2021 American Chemical Society

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