Hypercrosslinking: New approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules

URBAN, Jiří; F SVEC and JMJ FRECHET. Hypercrosslinking: New approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules. Journal of Chromatography A. Amsterdam: ELSEVIER SCIENCE BV, 2010, vol. 1217, No 52, p. 8212-8221. ISSN 0021-9673. Available from: https://doi.org/10.1016/j.chroma.2010.10.100.

Basic information

Original name

Hypercrosslinking: New approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules

Authors

URBAN, Jiří; F SVEC and JMJ FRECHET

Edition

Journal of Chromatography A, Amsterdam, ELSEVIER SCIENCE BV, 2010, 0021-9673

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Other information

Language

English

Type of outcome

Article in a journal

Confidentiality degree

is not subject to a state or trade secret

Impact factor

Impact factor: 4.194

DOI

https://doi.org/10.1016/j.chroma.2010.10.100

UT WoS

000285899400017

Keywords in English

Hypercrosslinked polymer monolith; Poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene); Reversed phase chromatography; Size-exclusion chromatography; Small molecules

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Abstract

In the original language

Monolithic polymers with an unprecedented surface area of over 600 m(2)/g have been prepared from a poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene) precursor monolith that was swollen in 1,2-dichloroethane and hypercrosslinked via Friedel-Crafts reaction catalyzed by ferric chloride. Both the composition of the reaction mixture used for the preparation of the precursor monolith and the conditions of the hypercrosslinking reaction have been varied using mathematical design of experiments and the optimized system validated. Hypercrosslinked monolithic capillary columns contain an array of small pores that make the column ideally suited for the high efficiency isocratic separations of small molecules such as uracil and alkylbenzenes with column efficiencies reproducibly exceeding 80,000 plates/m for retained compounds. The separation process could be accelerated while also improving peak shape through the use of higher temperatures and a ternary mobile phase consisting of acetonitrile, tetrahydrofuran, and water. As a result, seven compounds were well separated in less than 2 min. These columns also facilitate separations of peptide mixtures such as a tryptic digest of cytochrome c using a gradient elution mode which affords a sequence coverage of 93%. A 65 cm long hypercrosslinked capillary column used in size exclusion mode with tetrahydrofuran as the mobile phase afforded almost baseline separation of toluene and five polystyrene standards. (C) 2010 Elsevier B.V. All rights reserved.