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

J 2010

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 a JMJ FRECHET

Základní údaje

Originální název

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

Autoři

URBAN, Jiří, F SVEC a JMJ FRECHET

Vydání

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

Další údaje

Jazyk

angličtina

Typ výsledku

Článek v odborném periodiku

Utajení

není předmětem státního či obchodního tajemství

Impakt faktor

Impact factor: 4.194

DOI

http://dx.doi.org/10.1016/j.chroma.2010.10.100

UT WoS

000285899400017

Klíčová slova anglicky

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

Změněno: 12. 3. 2021 13:36, doc. RNDr. Jiří Urban, Ph.D.

Anotace

V originále

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.

Citovat

URBAN, Jiří, F SVEC a 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, roč. 1217, č. 52, s. 8212-8221. ISSN 0021-9673. Dostupné z: https://dx.doi.org/10.1016/j.chroma.2010.10.100.

@article{1751696,
   author = {Urban, Jiří and Svec, F and Frechet, JMJ},
   article_location = {Amsterdam},
   article_number = {52},
   doi = {http://dx.doi.org/10.1016/j.chroma.2010.10.100},
   keywords = {Hypercrosslinked polymer monolith; Poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene); Reversed phase chromatography; Size-exclusion chromatography; Small molecules},
   language = {eng},
   issn = {0021-9673},
   journal = {Journal of Chromatography A},
   title = {Hypercrosslinking: New approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules},
   volume = {1217},
   year = {2010}
}

TY  - JOUR
ID  - 1751696
AU  - Urban, Jiří - Svec, F - Frechet, JMJ
PY  - 2010
TI  - Hypercrosslinking: New approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules
JF  - Journal of Chromatography A
VL  - 1217
IS  - 52
SP  - 8212-8221
EP  - 8212-8221
PB  - ELSEVIER SCIENCE BV
SN  - 00219673
KW  - Hypercrosslinked polymer monolith
KW  - Poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene)
KW  - Reversed phase chromatography
KW  - Size-exclusion chromatography
KW  - Small molecules
N2  - 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.
ER  -

URBAN, Jiří, F SVEC a JMJ FRECHET. Hypercrosslinking: New approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules. \textit{Journal of Chromatography A}. Amsterdam: ELSEVIER SCIENCE BV, 2010, roč.~1217, č.~52, s.~8212-8221. ISSN~0021-9673. Dostupné z: https://dx.doi.org/10.1016/j.chroma.2010.10.100.

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