Koshy K T, Kaiser D G, VanDerSlik A L
J Chromatogr Sci. 1975 Feb;13(2):97-104. doi: 10.1093/chromsci/13.2.97.
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 X 10(4) 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.
0-(2,3,4,5,6-五氟苄基)羟胺盐酸盐用于制备在特定位置带有酮基的甾体肟；3,17和20-单酮；3,17和3,20-二酮。一些3-酮甾体具有受阻的17-羟基，这些羟基不易用全氟酐进行酯化，全氟酐是用于羟基甾体电子捕获气相色谱分析最常用的衍生化试剂。从所测试的每种化合物5纳克很容易制备出肟，对于睾酮，已证明从低至0.1纳克就能制备出衍生物。这些衍生物对气相色谱稳定，对电子捕获检测极其灵敏。灵敏度范围为每摩尔孕酮1.5×10⁴库仑。由于衍生物制备容易、在常用溶剂中的稳定性以及分析操作技术，该试剂将适用于通过电子捕获气相色谱对具有生物学意义的酮甾体进行微量分析。
