COUNTER-CURRENT DISTRIBUTION PROCEDURE FOR THE QUANTITATIVE-QUALITATIVE ANALYSIS OF SMALL AMOUNTS OF URINARY CORTICOSTEROIDS*

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Abstract
Introduction THE present paper is an extension of previous work on procedures for the qualitative-quantitative analysis of small samples of urinary steroids of adrenocortical and gonadal origin (1). It involves the use of countercurrent distribution discussed by Craig (2). The amount of thiosemicarbazide reactive material present is estimated by means of the thiosemicarbazide reaction which Evans and Gillam have shown to be useful for the detection of alpha-beta unsaturated ketones (3). ANALYTIC PROCEDURE 1. Reagents and apparatus: Thiosemicarbazide reagent (Eastman Kodak Company). A 0.1 molar thiosemicarbazide solution in 0.1 molar hydrochloric acid is prepared and filtered into a glass-stoppered bottle. It is stable at room temperature for several months. Ethanol, absolute (U. S. Industrial Chemicals Company) Chloroform, reagent grade. Sodium hydroxide, 0.1 N solution. Secondary butyl alcohol (Eastman Kodak Company, highest purity), redistilled in an all-glass apparatus. Iso-octane (2,2,4-trimethylpentane, pure grade 99 mol per cent; Phillips Petroleum Company, Chemical Products Division, Bartlesville, Oklahoma).

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