Abstract

The 3,20-bismethyloxime-11-diethylhydrogensilyl-17,21-cyclic diethylsilylene derivative of hydrocortisone (HC) was obtained by treating HC with O-methylhydroxylamine hydrochloride and then with N,O-bis(diethylhydrogensilyl)trifluoroacetamide. This derivative gave a single peak without resolution of its structural isomers. The electron-impact mass spectrum of the HC derivative was characterized by the appearance of an intense molecular ion peak and principal ion peak of [M — OCH 3 ] + at m / z 559. The detection limit was 10 pg with a signal-to-noise ratio of more than 10 when gas chromatography (GC)—selected ion monitoring was carried out at the molecular ion of m / z 590. On the other hand, GC—metastable peak monitoring, based on the metastable peak corresponding to the transition ions from m / z 590 to 559, showed a detection limit of ca . 10 pg with a signal-to-noise ratio of more than 5.

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