Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
38, Number 11, November 2000, pp. 477-482
Feasibility
of On-Line Supercritical Fluid Extraction of Steroids from Aqueous-Based Matrices
with Analysis via Gas Chromatography–Mass SpectrometryM.
Ashraf-Khorassani
Durability Inc., 1875 Pratt Dr., Blacksburg, VA 24060 L.T. Taylor*
Department of Chemistry, Virginia Tech, Blacksburg, VA 24061-0212
The solubility
of testosterone, boldenone, androstenone, etiocholanolone, and epitestosterone
are measured in pure supercritical CO2. Testosterone exhibited the highest solubility
in supercritical CO2. The solubility of all steroids except epitestosterone
increased by one order of magnitude with increasing pressure from 100 to 400
atm. Epitestosterone had the lowest solubility in supercritical CO2 and its
solubility was not affected by pressure. The extraction efficiency of steroids
from an aqueous saline environment exceeded 95%. Because of the partial solubility
of water in supercritical CO2, the addition of a moisture trap after the aqueous
vessel is necessary to prevent the plugging and deterioration of the gas chromatographic
(GC) column. It is demonstrated that on-line supercritical fluid extraction–GC–mass
spectrometry is feasible for the quantitative extraction and analysis of steroids
from both saline and urine solutions. However, it is determined that the adsorbent
vessel filled with Hydromatrix is not sufficient to trap all the moisture, and
after 3 to 4 extractions, the GC column efficiency lowered.
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