Dimethylisopropylsilyl ether derivatives in gas chromatography-mass spectrometry of some prostanoids : Application to the microdetermination of 15-ketoprostaglandin F formed by enzymatic conversion of PGF in vitro

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Abstract

Treatment of 15-ketoprostaglandin F (15-keto-PGF) with ethereal diazomethane at −78°C provided only the expected methyl ester (ME), without the formation of the pyrazoline adduct. The electron-ionization mass spectrum of the dimethylisopropylsilyl (DMiPS) ether derivative of 15-keto-PGF ME showed the molecular ion, and the characteristic fragment ion of [M−43]+ was of high abundance. The appearance of these ions in the high-mass region made it possible to determine trace amounts of 15-keto-PGF in biological specimens without any interference from endogenous substances. The detection limit for the DMiPS ether derivatives of 15-keto-PGF ME was 12 pg (signal-to-noise ratio = 10). The method was applied to the analysis of 15-keto-PGF obtained by the enzymatic conversion of PGF with 15-hydroxyprostaglandin dehydrogenase in vitro.

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