, Volume 51, Issue 11–12, pp 747–755 | Cite as

Characterization of a solventless injection interface for supercritical fluid chromatography

  • J. Y. Gao
  • C. E. Kibbey


Packed column supercritical fluid chromatography (SFC) is capable of highly efficient separations of drug-like molecules with les solvent consumption than HPLC. However, solute peaks in SFC are susceptible to broadening and distortion due to mismatch between the elution strength and viscosity of the injection solvent and the SFC mobile phase. The magnitude of solvent-induced band broadening increases as the elution strength and viscosity of the sample and mobile phase become more dissimilar and varies with the type of stationary phase used and the nature of the solute injected. A number of researchers have coupled supercritical fluid extraction with supercritical fluid chromatography in an attempt to remove solvent from injected samples, and thereby reduce peak broadening and distortion during SFC chromatography. While solventless injection is effective in overcoming solvent-induced band broadening in SFC, there have been few reports dealing with the optimization of the solvent removal process of this technique. In this work, we describe the influence of temperature, purge time, purging gas flow rate, stationary phase used in the sample precolumn, and injection solvent composition on solvent elimination and solute recovery.

Key Words

Supercritical fluid chromatography Solventless injection Solvent-induced band broadening 


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  1. [1]
    M. Tsimidou, R. Macrae, J. Chromatogr.,285, 178, (1984).CrossRefGoogle Scholar
  2. [2]
    M. Tsimidou, R. Macrae, J. Chromatogr. Sci.,23, 155, (1985).Google Scholar
  3. [3]
    F. Khachik, G. R. Beecher, J. T. Vanderslice, G. Furrow, Anal. Chem.,60, 807, (1988).CrossRefGoogle Scholar
  4. [4]
    D. Cherrak, E. Guernet, P. Cardot, C. Herrenknecht, M. Czok, Chromatographia,46, 647 (1997).CrossRefGoogle Scholar
  5. [5]
    R. C. Castells, C. B. Castells, M. A. Castillo, An. CIDEPINT,1997–1998, 111, (1998).Google Scholar
  6. [6]
    T. A. Berger, J. F. Deye, Supercritical Fluid Technology, inF. V. Bright, M. E. P. McNally, Eds., ACS Symposium Series 488, American Chemical Society, Washington, DC, 1992, Chapter 11.Google Scholar
  7. [7]
    T. A. Dean, C. F. Poole, J. High Res. Chromatogr.,12, 773, (1989).CrossRefGoogle Scholar
  8. [8]
    G. Cretier, R. Majdalani, J. L. Rocca, Chromatographia,30, 645, (1990).CrossRefGoogle Scholar
  9. [9]
    J. W. Oudsema, C. F. Poole, J. High Res. Chromatogr.,15, 65, (1992).CrossRefGoogle Scholar
  10. [10]
    G. Cretier, R. Majdalani, J. Neffati, J. L. Rocca, Chromatographia,38, 330, (1994).CrossRefGoogle Scholar
  11. [11]
    Y. Hirata, Y. Kawaguchi, K. Kitano, Chromatographia,40, 42, (1995).CrossRefGoogle Scholar
  12. [12]
    P. Jandera, G. Guiochon, J. Chromatogr.,588, 1, (1991).CrossRefGoogle Scholar

Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 2000

Authors and Affiliations

  • J. Y. Gao
    • 1
  • C. E. Kibbey
    • 1
  1. 1.Parke-Davis Pharmaceutical ResearchDivision of Warner-Lambert CompanyAnn ArborUSA

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