QUANTITATION OF C19O2 AND C21O2 STEROID MONO- AND DISULFATES IN HUMAN BILE

A method is described for the determination of the mono-sulfates of androsterone, etiocholanolone, 3a-hydroxyandrost-5-en-17-one, dehydroepiandrosterone, pregnenolone, 5α-pregnane-3α, 20α-diol, 5β-pregnane-3α,20α-diol and pregn-5-ene-3β, 20α-diol, and the disulfates of 5α-androstane-3α, 17α-diol, 5α-androstane-3a, 17β-diol, androst-5-ene-3β, 17α-diol, androst-5-ene-3β, 17β-diol, 5a-pregnane-3α,20α-diol, 5β-pregnane-3α,20α-diol and pregn-5--ene-3β, 20α-diol in human bile. After extraction, the steroid monosulfate and disulfate fractions are obtained from bile by chromatography on Sephadex LH-20. After solvolysis the steroids are fractionated on silicic acid and analyzed by gas chromatography as trimethyl silyl ethers on QF-1 and SE-30 columns. The specificity of the method was established by mass spectrometric analysis of the effluent from the GLC columns. The total concentration of the C19O2 and C21O2 steroids measured was 320 μg/100 ml in a fistula bile pool from males and 780 μg/100 ml in a gall-bladder bile pool from females. Of these total amounts, the steroid diols in the disulfate fraction form 79 % and 68 %, respectively, and the 17-ketosteroids 15% and 19%, respectively. © 1968.