Monolithic poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for simultaneous separation of low- and high-molecular-weight compounds.
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 alpha,alpha'-azoisobutyronitrile (AIBN) as initiator. Polymerisations were accomplished in 200 microm ID fused silica capillaries at 65 degrees 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 mum 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 (approximately 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 micro-HPLC towards a huge range of analytes of different chemistries and molecular sizes.
Greiderer
Andreas
A
Institute of Analytical Chemistry and Radiochemistry, University of Innsbruck, 6020 Innsbruck, Austria.
Ligon
S Clark
SC
Huck
Christian W
CW
Bonn
Günther K
GK
D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation*; D019075:Electrophoresis, Capillary / Q000295:instrumentation*; D004980:Ethane / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D015394:Molecular Structure; D008970:Molecular Weight; D009841:Oligonucleotides / Q000302:isolation & purification; D010636:Phenols / Q000737:chemistry; D011108:Polymers / Q000138:chemical synthesis / Q000737:chemistry*; D016062:Porosity; D011312:Pressure; D011506:Proteins / Q000302:isolation & purification; D015203:Reproducibility of Results; D012997:Solvents; D014753:Vinyl Compounds / Q000138:chemical synthesis / Q000737:chemistry*
D009841:Oligonucleotides; D010636:Phenols; D011108:Polymers; D011506:Proteins; D012997:Solvents; D014753:Vinyl Compounds; D004980:Ethane