1972 年 92 巻 9 号 p. 1157-1161
Gas chromatographic method for determination of urinary metabolites derived from an officinal dose of 3-deoxyestrone (I) and 16α-chloroestrone methyl ether (II) hat been devised. Separation of each of three principal metabolites was satisfactorily attained when they were transformed into the trifluoroacetyl derivatives and then subjected to gas chromatography under the appropriate column conditions (Table I). The structures of the metabolites were confirmed by gas chromatography-mass spectrometry (Fig. 2). Preliminary purification by thin-layer chromatography proved to be effective for removal of interference due to undesirable substances, less and more polar than the metabolites. The calibration curve for quantitation of each metabolite was constructed. employing androst-5-ene-3β, 16β, 17β-triol tris (trifluoroacetate) as an internal standard. The amount of the metabolites excreted in urine after oral administration of I and II to man was determined by the procedure thus established.