Use of Gas-Liquid Chromatography With Glass Capillary Columns For Steroid Trace Analysis In Tissues

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Abstract
Performances of a glass capillary column with an all-glass solid injection system have been evaluated for the analysis of steroid hormones with regard to separation and reproducibility of retention and sensitivity. O-methyloxime-trimethylsilyl derivatives have been prepared from 25 steroids of the C19 and the C21 series for which methylene unit values have been measured on an apolar phase (SE-30) with optimized accuracy. High efficiency of the column leads to the complete resolution of stereoisomeric steroids such as the four tetrahydrocorticosterone isomers and to the separation of the syn and anti isomers of the 3-methoxime-Δ-4-steroids unresolved on an apolar packed column. After preliminary fractionation of rat adrenal and liver extracts by thin-layer chromatography, corticosterone metabolites have been separated and detected in the range of 1–50 ng with a flame ionization detector. The configuration of tetrahydrocorticosterone isomers has been shown to be dependent on tissue, age and sex of the rat. This technique can help in the study of corticosterone biosynthesis regulation especially as used in association with gas chromatographic-mass spectrometric methods.

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