Synthesis and chromatographic properties of monolithic columns based on copolymers of divinylbenzene and ethylvinylbenzene with hydroxyalkyl methacrylates
Keywords:
monolithic column, divinylbenzene, hydroxyalkyl methacrylate, HPLC.
Abstract
Monolithic stationary phases based on copolymers of divinylbenzene (DVB) and
ethylvinylbenzene (EVB) with various hydroxyalkyl methacrylates were synthesized via thermally
initiated free-radical polymerization inside glass tubes with dimensions of 150 × 3 mm. The use of
hydroxybutyl methacrylate instead of hydroxyethyl methacrylate (HEMA) was found to increase the
column permeability by a factor of 1,6 with 5–10% drop in efficiency. The effect of column temperature
on separation using poly(DVB-co-EVB-co-HEMA) monolith was studied. Raising the temperature from
25°C to 80°C increased the efficiency of the column and maximum flow rate of the mobile phase and
reduced the influence of retention factor on peak broadening. At 80°C and velocities up to 3,7 mm/s the
efficiency for alkylbenzenes was 19000–20000 plates/m
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2.Svec F. Porous polymer monoliths: amazingly wide variety of techniques enabling
their preparation // J. Chromatogr. A. 2010. V. 1217. № 6. P. 902–924.
3.Vlakh E.G., Tennikova T.B. Applications of polymethacrylate-based monoliths in
high-performance liquid chromatography // J. Chromatogr. A. 2009. V. 1216. № 13. P.
2637–2650.
4.Urban J., Svec F., Fréchet J.M.J. Hypercrosslinking: new approach to porous polymer
monolithic capillary columns with large surface area for the highly efficient separation of
small molecules // J. Chromatogr. A. 2010. V. 1217. № 52. P. 8212–8221.
5.Nischang I., Teasdale I., Brüggemann O. Towards porous polymer monoliths for the
efficient, retention-independent performance in the isocratic separation of small molecules
by means of nano-liquid chromatography // J. Chromatogr. A. 2010. V. 1217. № 48. P.
7514–7522.
6.Greiderer A., Trojer L., Huck C.W., Bonn G.K. Influence of the polymerisation time on
the porous and chromatographic properties of monolithic poly(1,2-bis(pvinylphenyl))
ethane capillary columns // J. Chromatogr. A. 2009. V. 1216. № 45. P. 7747–
7754.
7.Викторова Е.Н., Канатьева А.Ю., Королев А.А., Курганов А.А. Монолитные
капиллярные колонки на основе дивинилбензола в капиллярной жидкостной
хроматографии // Журн. физич. химии. 2007. Т. 81. № 3. С. 507–511.
8.Матусова С.М., Иванова К.И., Дьячков И.А., Смоленков А.Д., Пирогов А.В.,
Шпигун О.А. Полиалкилметакрилатные монолитные колонки для ВЭЖХ // Изв. АН.
Сер. химич. 2008. № 12. C. 2503–2509.
9.Trojer L., Lubbad S.H., Bisjak C.P., Wieder W., Bonn G.K. Comparison between
monolithic conventional size, microbore and capillary poly(p-methylstyrene-co-1,2-bis(pvinylphenyl)
ethane) high-performance liquid chromatography columns. Synthesis,
application, long-term stability and reproducibility // J. Chromatogr. A. 2007. V. 1146. №
2. P. 216–224.
10. Mayr B., Hölzl G., Eder K., Buchmeiser M.R., Huber C.G. Hydrophobic, pellicular,
monolithic capillary columns based on cross-linked polynorbornene for biopolymer
separations // Anal. Chem. 2002. V. 74. № 23. P. 6080–6087.
11. Smirnov K.N., Dyatchkov I.A., Telnov M.V., Pirogov A.V., Shpigun O.A. Effect of
monomer mixture composition on structure and chromatographic properties of
poly(divinylbenzene-co-ethylvinylbenzene-co-2-hydroxyethyl methacrylate) monolithic
rod columns for separation of small molecules // J. Chromatogr. A. 2011. V. 1218. № 30.
P. 5010–5019.
12. Huo Y., Schoenmakers P.J., Kok W.T. Efficiency of methacrylate monolithic
columns in reversed-phase liquid chromatographic separations // J. Chromatogr. A. 2007.
V. 1175. № 1. P. 81–88.
Published
2019-11-22
How to Cite
Smirnov, K. N., Dyatchkov, I. A., Pirogov, A. V., & Shpigun, O. A. (2019). Synthesis and chromatographic properties of monolithic columns based on copolymers of divinylbenzene and ethylvinylbenzene with hydroxyalkyl methacrylates. Sorbtsionnye I Khromatograficheskie Protsessy, 12(2). Retrieved from https://journals.vsu.ru/sorpchrom/article/view/1773
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