Monolithic capillary columns based on pentaerythritol acrylates for molecular‐size‐based separations of synthetic polymers

Polymethacrylate-based monolithic capillary columns, prepared by γ-radiation-induced polymerization, were used to optimize the experimental conditions (nature of the organic modifiers, the content of trifluoroacetic acid and the column temperature) in the separation of nine standard proteins with different hydrophobicities and a wide range of molecular weights. Because of the excellent permeability of the monolithic columns, an ion-pair reversed-phase capillary liquid chromatography with high-resolution mass spectrometry method has been developed by coupling the column directly to the mass spectrometer without a flow-split and using a standard electrospray interface. Additionally, the high working flow and concomitant high efficiency of these columns allowed us to employ a longer column (up to 50 cm) and achieve a peak capacity value superior to 1000. This work is motivated by the need to develop new materials for high-resolution chromatographic separation that combine chemical stability at elevated temperatures (up to 75°C) and a broad pH range, with a high peak capacity value. The advantage of the γ-ray-induced monolithic column lies in the batch-to-batch reproducibility and long-term high-temperature stability. Their proven high loading capacity, recovery, good selectivity and high permeability, moreover, compared well with that of a commercially available poly(styrene-divinylbenzene) monolithic column, which confirms that such monolithic supports might facilitate analysis in proteomics.

Section: Introductionmentioning

confidence: 99%

Separation of intact proteins on γ‐ray‐induced polymethacrylate monolithic columns: A highly permeable stationary phase with high peak capacity for capillary high‐performance liquid chromatography with high‐resolution mass spectrometry

Simone

Pierri

Foglia

et al. 2015

“…The smaller molecules penetrate into these pores as they pass through the column and they are temporary retained, while larger ones are not, and they flow more rapidly down the length of the column. Finally, molecules with different molecular sizes are separated . Comparing with other chromatographic techniques the analysis time is considerably longer and usually takes up to 20–60 min per run.…”

Section: Introductionmentioning

confidence: 99%

Linear polymer separation using carbon‐nanotube‐modified centrifugal filter units

Krawczyk

Marian

Pawlyta

2015

The separation of linear polymers such as polysaccharides and polyethylene glycol was performed with modified commercial centrifugal filter units. The deposition of a 0.16-0.35 μm layer of modified carbon nanotubes prevented permeation of linear polymers of molecular weight higher than 20 000 Da through the membrane. It allowed facile purification of solution of 0.1 g of polymer samples from small molecules within 25 min by using a bench-top centrifuge. The structure of modified carbon nanotubes was optimized in order to achieve good adhesion to the low binding regenerated cellulose surface and low solubility in aqueous solutions after deposition. The best modification of carbon nanotubes was oxidation and subsequent amide formation of diethanolamine. Introduction of acetic acid groups using sodium chloroacetate worked equally well. The modified filter could be used multiple times without the decrease of the efficiency. The carbon nanotubes layer was stable in aqueous solutions in a pH range of 1-7. The proposed method provides a convenient way of purification of modified polymers in research areas such as drug delivery or macromolecular probes synthesis.

Monolithic thin‐layer chromatography plates with covalently bonded matrix for hyphenation with matrix‐assisted laser desorption/ionization

Kucherenko

Kanat’eva

Kurganov

et al. 2018

Self Cite

Monolithic layers prepared by the copolymerization of ethylene dimethacrylate and glycidyl methacrylate and deposited onto the surface of glass and silicon plates were investigated as thin‐layer chromatography separation media in hyphenated thin‐layer chromatography with matrix‐assisted laser desorption/ionization mass spectrometry (MALDI‐MS) analysis. Varying composition of the polymerization mixture and polymerization conditions layers of different porosities and MALDI‐MS compatibility were synthesized. Compatibility with MALDI‐MS was tested using polyethylene glycol and it was demonstrated that layers prepared without glycidyl methacrylate are not compatible with MALDI‐MS and do not allow obtaining any mass spectra. Best results were achieved with layers containing 19 to 29% glycidyl methacrylate. These layers allow the measurement of mass spectra without additional depositing matrix compounds supplying mass spectra almost “clean” in low molar mass range.