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

Jiri Urban, Frantisek Svec, Jean M.J. Fréchet*

*Corresponding author for this work

    Research output: Contribution to journalArticlepeer-review

    151 Scopus citations

    Abstract

    Monolithic polymers with an unprecedented surface area of over 600m2/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 80,000plates/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 2min. 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 65cm 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.

    Original languageEnglish (US)
    Pages (from-to)8212-8221
    Number of pages10
    JournalJournal of Chromatography A
    Volume1217
    Issue number52
    DOIs
    StatePublished - Dec 24 2010

    Keywords

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

    ASJC Scopus subject areas

    • Analytical Chemistry
    • Biochemistry
    • Organic Chemistry

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