Abstract
Five different estrogen monoglucuronides have been separated at least partially by gas chromatography of the permethyl derivatives on OV-17 columns either isothermally or with temperature programming. The permethyl derivatives are formed quantitatively with a greater than tenfold excess of the methylsulfinylmethide carbanion and methyl iodide. On the other hand, quantitative derivatization (>98%) of the aglycones, estradiol and estriol, is effected only with a thirtyfold or greater excess of the carbanion. Mono-, di-, and trimethyl derivatives are found and all have characteristic mass spectra. The mass spectra of the permethylated glucuronides are also clearly different. All spectra contain molecular ions and fragment ions due to the permethylated glucuronic acid moiety, the aglycones, and M-CH 3OH. This data is being applied to the analysis of intact estrogen glucuronides in body fluids.
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