Summary
Polyethylene oxide (PEO)-based polymers with hydroxy, methoxy, and aminopropoxy terminal groups were coated on diol functionalized and hexamethyldisilazane end-capped silica particles. Proton-donor and proton-acceptor test solutes, including carboxylic acids, hydroxy-containing compounds, arylamines, and alkylamines were used to evaluate the chromatographic performances of these polymer coated particles under SFC conditions with neat CO2 as mobile phase. It was found that the particles coated with hydroxy-terminated PEO were suitable for the separation of proton-donor compounds such as hydroxy-containing compounds and carboxylic acids, and the particles coated with aminopropoxy-terminated PEO could be used for the separation of amines. That is, the proton-accepting stationary phase is suitable for the separation of proton accepting solutes, including strong basic alkylamines (pKb≈4), using neat CO2 as mobile phase, while the protondonating stationary phase is suitable for the separation of proton-donating compounds such as carboxylic acids (pKa≈4). Hydrogen bond basicity was found to be a critical factor for the chromatography of basic amines. Low volatility acidic and basic drugs were chromatographed using the new stationary phases. The stability of the PEO coated particles was determined by measuring the loss of organic carbon under SFC conditions. It was found that approximately 18 % of the coating (average molecular weight of 15,000) was washed out of the particles by supercritical CO2 after 7 h at 350 atm and 50°C
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
K. K. Unger, “Porous Silica”, Elsevier, Amsterdam, 1979.
C. Horváth, “Techniques in Liquid Chromatography” F. Simpson, Ed., John Wiley & Sons, 1982, Chapter 10.
Y. Shen, M. L. Lee, Chromatographia41, 665 (1995).
Y. Shen, M. L. Lee, J. Microcol. Sep. in press.
H. Figge, A. Deege, J. Köhler, G. Schomburg, J. Chromatogr.351, 393 (1986).
Y. Shen, M. L. Lee, “Seventeenth International Symposium on Capillary Chromatography and Electrophoresis”, Wintergreen, VA, May 7–11, 1995, p. 498.
H. Traitler, L. Kolarovic, A. Sorio, J. Chromatogr.279, 69 (1983).
M. V. Russo, G. C. Goretti, A. Liberti, J. High Resolut. Chromatogr./Chromatogr. Commun.8, 535 (1985).
M. Cigánek, M. Dressler, J. Teply, J. Chromatogr.588, 225 (1991).
M. M. Daniewski W. A. Aue, J. Chromatogr.147, 119 (1978).
I. Choma, A. L. Dawidowicz, R. Dobrowolski, S. Pikus, J. Chromatogr.641, 205 (1993).
I. Choma, A. L. Dawidowicz, R. Dobrowolski, S. Pikus, J. Chromatogr.641, 211 (1993).
H. E. Persinger, J. T. Shank, J. Chromatogr. Sci.11, 190 (1973).
M. L. Lee, K. E. Markides, Eds., “Analytical Supercritical Fluid Chromatography and Extraction”, Provo, Utah, 1990, Chap. 2.
K. M. Payne, B. J. Tarbet, K. E. Markides, M. L. Lee, Anal. Chem.62, 1379 (1990).
A. Malik, W. Li, M. L. Lee, J. Microcol. Sep.5, 361 (1993).
D. J. Eatough, B. Sedar, L. Lewis, L. D. Hansen, E. A. Lewis, R. J. Farber, Aerosol Sci. Techn.10, 438 (1989).
E. Ibanez, J. Tabera, G. Reglero, M. Herraiz, Chromatographia40, 448 (1995).
O. Gyllenhaal J. Vessman, J. Chromatogr.516, 415 (1990).
Y. Shen, J. S. Bradshaw, M. L. Lee, Chromatographia43, 53 (1996).
M. H. Abraham, P. P. Duce, P. L. Grellier, D. V. Prior, J. J. Morris, P. J. Taylor, Tetrahedron Lett.29, 1587 (1988).
M. H. Abraham, Chem. Soc. Rev.22, 73 (1993).
D. K. Dandge, J. P. heller, K. V. Wilson, Ind. Eng. Chem. Prod. Res. Dev.24, 162 (1985).
F. David, P. Sandra, J. High Resolut. Chromatogr./Chromatogr. Commun.11, 897 (1988).
A. C. Legon, Chem. Soc. Rev.22, 153 (1993).
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Shen, Y., Lee, M.L. End-functionalized polyethylene oxide coated silica particles for packed capillary column supercritical fluid chromatography. Chromatographia 43, 373–379 (1996). https://doi.org/10.1007/BF02271014
Received:
Revised:
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF02271014