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0-(2,3,4,5,6-Pentafluorobenzyl)Hydroxylamine Hydrochloride as a Sensitive Derivatizing Agent for the Electron Capture Gas Liquid Chromatographic Analysis of Keto Steroids
Ist Teil von
Journal of chromatographic science, 1975-02, Vol.13 (2), p.97-104
Ort / Verlag
United States: Oxford University Press
Erscheinungsjahr
1975
Link zum Volltext
Quelle
MEDLINE
Beschreibungen/Notizen
0-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride was used to prepare oximes of steroids with keto groups in selected positions; 3,17 and 20-monoketo; 3,17 and 3,20-diketo. Some of the 3-keto steroids had hindered 17-hydroxyl groups which were not readily amenable to esterification with perfluoroanhydrides, the most commonly used derivatizing agents for electron capture gas chromatographic analysis of hydroxy steroids. The oximes were readily prepared from 5 ng of each of the compounds tested, and with testosterone it was demonstrated that the derivative could be prepared from as little as 0.1 ng. The derivatives were stable to gas chromatography and extremely sensitive to electron capture detection. The sensitivity ranged from 1.5 × 104 coulombs per mole of androsterone to 9.6 × 104 coulombs per mole of progesterone. Because of the ease of preparation of the derivatives, their stability in common solvents and analytical manipulative techniques, the reagent would be suitable for the micro analysis of biologically significant keto steroids by electron capture gas chromatography.