Separation of Steroid Hormones and Their Metabolites by Partition Type Chromatography

Partition Chromatography Of Steroids

“…For the isolation of 16-epiestriol from pregnancy urine Marrian and Bauld Boscott (52,53) devised partition systems of toluene and absolute ethanol or methanol by separating the mixture into two layers with addition of lithium chloride or calcium chloride. A similar situation may exist in the "partition type" silica gel columns of Katzenellenbogen, Dobriner, and Kritchevsky (216), if they are indeed partition columns. Absolute ethanol was used as the stationary phase and dichloromethane containing ethanol as the mobile phase for the fractionation of the acetates of adrenal steroids.…”

“…For the chromatography of adrenal steroids on filter paper impregnated with 1,2-propanediol, 1,2-dichloroethane-toluene (3:7) has also been used (98, 154). On formamide-impregnated columns adrenal steroids have been chromatographed with benzene-isooctane (22) or with cyclohexane-benzene or cyclohexane (216) as the mobile phase. Digitoxin preparations were analyzed on formamide columns with benzenechloroform as the eluant (25,24).…”

Steroidal Sapogenins. XXII.2 Conversion of Hecogenin Acetate to a Hecololactone Derivative with the Adrenal Cortical Hormone Side Chain via Allopregnane-3β,17α,21-triol-12,20-dione Diacetate

“…of ethanol. 21 The elution was carried out with 98% dichloromethane-2% ethanol moving phase. The product was eluted very quickly in less than 100 ml.…”

“…1C.10 Using II, m.p. 130-131°, as starting material we obtained by monobromination and acetolysis allopregnane-3/3,17 a, 21 -triol-12,20-dione 3,21-diacetate. This substance, in the presence of sulfuric acid catalyst, consumed in about 70 hours one equivalent of perbenzoic acid to form 12-carboxy-12,13-seco-allopregnane-3ß, 13 , 17 , 21-tetrol-(7) This substance was the main constituent of the mixture obtained by Stobaugh and Mueller in some experiments (private communication).…”

Isolation From Urine and Synthesis of Tetrahydrocortisone Glucuronoside

“…4 The crude glucuronoside obtained from tubes 12 through 25 following the countercurrent distribution was hydrolyzed with /3-glucuronidase. The recovered neutral fraction was acetylated and chromatographed (3) to give 3 ,20/3,21 -triacetoxy-17 -hydroxypregnane-11-one (/3-cortolone triacetate) (4) m.p. 205-206°u ncor.…”