Comparison between monolithic conventional size, microbore and capillary poly(p-methylstyrene-co-1,2-bis(p-vinylphenyl)ethane) high-performance liquid chromatography columns

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.

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“…Again, the tremendously increased surface area [14] can be explained by the presence of an enhanced fraction of mesopores and small macropores.…”

Section: Porosity Of Bvpe Monolithmentioning

confidence: 97%

“…The second region illustrates the flow-channels of the polymer and is responsible for the high permeability of BVPE support material. As a consequence of the high inter-microglobule porosity as well as the enhanced fraction of pores, the total porosity of the polymer of 81% is comparatively high [14].…”

Section: Porosity Of Bvpe Monolithmentioning

confidence: 99%

Monolithic poly(1,2‐bis(p‐vinylphenyl)ethane) capillary columns for simultaneous separation of low‐ and high‐molecular‐weight compounds

Greiderer

Huck

Bonn³

2009

J of Separation Science

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“…Unlike capillary work, the user has no option to cut out or remove less-optimal sections of the separation channels in a microdevice. The high mechanical stability with little swelling exhibited by the MS/BVPE monoliths have been extensively described elsewhere [21,29] and these qualities were borne out inside the microdevices.…”

Section: Chip Wall Preparation and Monolith Fabricationmentioning

confidence: 99%

“…The polymeric monoliths used in this work were MS/ BVPE-based monoliths described extensively in work of Trojer et al [21,29]. The crosslinker (BVPE) was synthesized [21] and recrystallized from methanol to give brilliant white flakes (80% yield).…”

Section: Chemical Preparation Of Crosslinker and Monolithic Chip Chanmentioning

confidence: 99%

Microfluidic HPLC‐Chip devices with integral channels containing methylstyrenic‐based monolithic media

Robotti¹,

Yin

Brennen

et al. 2009

J of Separation Science

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Polyimide HPLC-Chip devices containing poly(methylstyrene-bis-p-vinylphenyl)ethane (MS/BVPE) stationary phase within the device channels and with wall attachment were prepared by thermally initiated free radical polymerization. The microfluidic devices were coupled to both UV and MS detectors. The potential of the MS/BVPE monolith as an alternative separation media within chip devices was investigated by side-by-side comparisons to particulate media within commercial devices. The chromatographic behavior of this stationary phase was comparable to particulate media for separations of proteins as the average peak width at half-height was equal (6.2 s) for a separation within 8 min under gradient elution conditions. The ability to control the porosity characteristics of the MS/BVPE monolith with changes in polymerization time also extended its utility into small analyte (< 500 Da) applications, although more optimization is needed to match conventional RP media for these applications. The good mechanical stability of the MS/BVPE monolith within the microdevices enabled excellent run-to-run repeatability (%RSD retention time (< or = 0.16) and chip-to-chip reproducibility (%RSD retention time (1.4). The use of this material within enrichment channels also shows its potential value in more complex work flows.

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“…Polymeric materials are in one hand helpful in SPE [11][12][13] and on the other hand they have also attracted attention as a starting material in immobilized affinity chromatographic (IMAC) based proteomics (MELDI) as well as a reactor for enzymatic digestion [14]. Monolithic capillary columns synthesized by copolymerizing bis(vinylphenylethane) and methylstyrene have been shown to be highly suitable for the separation of even low-(phenolic compounds, flavonoids) and high molecular weight analytes (peptides, proteins, oligonucleotides) by l-LC [15,16]. An overview on the different kinds of investigated stationary phases synthesized in our laboratory, and their application is provided in Fig.…”

Section: Introductionmentioning

confidence: 99%

Infrared Spectroscopy: A Novel Tool for the Physicochemical Characterization of Particulate, Monolithic and Coated Stationary Phases

Huck

Bittner

2011

Chromatographia

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The design of novel stationary phases is a permanent demanding challenge in chromatographic and electrophoretic separation science to enable analysis with enhanced selectivity, specificity and speed. Therefore, the characterization of chemical and physical properties is next to calculation of chromatographic parameters essential. Conventionally, column performance is checked by a test run which only enables to prove efficiency column by column. Chemical parameters including surface coverage is normally analyzed by burning combustion or frontal analysis, physical parameters including particle size, pore size, pore volume and surface area by SEM, mercury intrusion porosimetry and Brunauer Emmett Teller. All these methods are extremely time consuming, invasive and require, beside special equipment, some specially trained lab staff. In order to enable a fast high-throughput control of chemical and physical parameters we introduced near-infrared spectroscopy (NIRS, 4,000-10,000 cm -1 ) as a non-invasive, easy-to-handle technology enabling simultaneous analysis within only a few seconds at higher precision than the conventional applied methods. The method is applicable to porous/non-porous silica gel, carbon-based nano-materials (e.g. fullerenes), polymer beads, monoliths for solidphase extraction, liquid chromatography, micro-liquid chromatography, material-enhanced laser desorption ionization and coated capillaries for capillary electrophoresis and capillary electrochromatography. Different carriers themselves and their kind of chemical derivatization (reversed-phase, normal-phase, ion-exchanger, immobilized affinity chromatography, affinity, endcapping) can be determined by applying principal component analysis of spectra recorded. Partial least square regression enables the determination of physical parameters particle size, pore size, pore volume, porosity, total porosity and surface area with one single measurement in an established quantitative model. For a detailed investigation NIRS imaging, which benefits from the combination of a NIR spectrometer with a microscope, allows to analyze materials of interest with resolution down to 4 lm. For the optimized design of polymeric phases real-time in situ monitoring to control polymerization progress can be highly helpful. In this article, the advantages of this novel infrared-based method for the fast high-throughput quality control are introduced.

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Comparison between monolithic conventional size, microbore and capillary poly(p-methylstyrene-co-1,2-bis(p-vinylphenyl)ethane) high-performance liquid chromatography columns

Cited by 40 publications

References 32 publications

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) capillary columns for simultaneous separation of low‐ and high‐molecular‐weight compounds

Microfluidic HPLC‐Chip devices with integral channels containing methylstyrenic‐based monolithic media

Infrared Spectroscopy: A Novel Tool for the Physicochemical Characterization of Particulate, Monolithic and Coated Stationary Phases

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