Determination of pregnane-17,21-diol-20-ones in human urine.

Treatment of urine or of a urine extract with periodate followed by treatment of the acidic oxidation products with sodium bismuthate gave a mixture of neutral end products consisting only or predominantly of 17-oxoandrostanes derived from the corresponding urinary pregnane-17,21-diol-20-ones. The mixture of end products was resolved by gas-liquid or paper chromatography. The latter technique was used to determine cortisol secretion rates and the results were found to be in reasonable agreement with those obtained by a double-isotope method. Gas-liquid-chromatographic characterization of steroidal 4-en-3-ones is described.