By Erich Heftmann (Eds.)
ISBN-10: 044441441X
ISBN-13: 9780444414410
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Extra resources for Chromatography of Steroids
Example text
D means that the compound decomposes. 36 GAS CHROMATOGRAPHY TMS and TFA derivatives of Cla and CI9 steroids. The combination of stationary phases combines the fractionation according to molecular weight by the nonselective, nonpolar silicone rubber with the selectivity of the polar ester phase. An improved version of this binary mixture, in which tetramethylcyclobutanediol adipate (TMCBA) replaces NGS, is stable at temperatures up to 25OoC for four days or 240°C for seven days [854]. 2 shows the relative retention times of a number of steroid derivatives, as determined with both argon-ionization and electron-capture detectors on a 6-ft.
For GC, hydroxylic steroids are often converted to trimethylsilyl (TMS) ethers (see p. 31). These ethers are easily purified by TLC, and even nanogram quantities of steroids with one or more alcohol groups may be recovered quantitatively [ 1 13,1241. Suitable developing solvents are: cyclohexane-ethyl acetate (9: l), benzene, chloroform, and cyclohexanechloroform (7:3 or 4: 1). A spray reagent of 1% Ce(S04)2 in 10%H2SO4 may be used for detection, and diethyl ether is a good eluent for recovery.
Instead of silica gel, porous glass (pore diameter 30-40 A) can be affixed t o glass plates, but this has no advantage, because steroids tend to streak and to give more diffuse zones on porous-glass layers [696]. However, by mixing one part of silica gel with two to five parts of glass powder of similar particle size, applying this mixture in a slurry of solvent to glass plates, and then heating them at 450--750”C for a few minutes, one can obtain thin layers with several advantages over plates prepared with other binders [820].
Chromatography of Steroids by Erich Heftmann (Eds.)
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