Monolithic poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for simultaneous separation of low- and high-molecular-weight compounds
✍ Scribed by Andreas Greiderer; S. Clark Ligon Jr.; Christian W. Huck; Günther K. Bonn
- Publisher
- John Wiley and Sons
- Year
- 2009
- Tongue
- English
- Weight
- 964 KB
- Volume
- 32
- Category
- Article
- ISSN
- 1615-9306
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✦ Synopsis
Abstract
Monolithic poly(1,2‐bis(p‐vinylphenyl)ethane (BVPE)) capillary columns were prepared by thermally initiated free radical polymerisation of 1,2‐bis(p‐vinylphenyl)ethane in the presence of inert diluents (porogens) and α,α′‐azoisobutyronitrile (AIBN) as initiator. Polymerisations were accomplished in 200 μm ID fused silica capillaries at 65°C and for 60 min. Mercury intrusion porosimetry measurements of the polymeric RP support showed a broad bimodal pore‐size‐distribution of mesopores and small macropores in the range of 5–400 nm and flow‐channels in the μm range. N~2~‐adsorption (BET) analysis resulted in a tremendous enhancement of surface area (101 m^2^/g) of BVPE stationary phases compared to typical organic monoliths (˜20 m^2^/g), indicating the presence of a considerable amount of mesopores. Consequently, the adequate proportion of both meso‐ and (small) macropores allowed the rapid and high‐resolution separation of low‐molecular‐weight compounds as well as biomolecules on the same monolithic support. At the same time, the high fraction of flow‐channels provided enhanced column permeability. The chromatographic performance of poly(1,2‐bis(p‐vinylphenyl)ethane) capillary columns for the separation of biomolecules (proteins, oligonucleotides) and small molecules (alkyl benzenes, phenols, phenons) are demonstrated in this article. Additionally, pressure drop versus flow rate measurements of novel poly(1,2‐bis(p‐vinylphenyl)ethane) capillary columns confirmed high mechanical robustness, low swelling in organic solvents and high permeability. Due to the simplicity of monolith fabrication, comprehensive studies of the retention and separation behaviour of monolithic BVPE columns resulted in high run‐to‐run and batch‐to‐batch reproducibilities. All these attributes prove the excellent applicability of monolithic poly(1,2‐bis(p‐vinylphenyl)ethane) capillary columns for μ‐HPLC towards a huge range of analytes of different chemistries and molecular sizes.