The Analysis of Digitoxin Tablets

Partition Chromatography Of Steroids

“…Progesterone (88,417,93), 17-ketosteroids (211), estrogens (40,60,151), adrenocortical hormones (22,182,197,276), bile acids (278,286,394), and cardiac glycosides (23,24,25) have been determined by various methods after column chromatography.…”

“…Subsequently, Morris and Williams (276) published a method for the determination of minute amounts of individual adrenocortical hormones by chromatography on two partition columns of Hyfio Supercel. The first column, which contained 25 per cent aqueous ethanol as the stationary phase and toluene as the mobile phase, gave a fore-fraction of dehydrocorticosterone, corticosterone, and 17-hydroxydeoxycorticosterone (11-deoxycorticosterone was not tested) and then two fractions, containing, in order, 11 -dehydro-17-hydroxycorticosterone and 17-hydroxycorticosterone.The fore-fraction was separated byrechromatographing on a second column with 1,2-ethanediol as the stationary phase and petroleum ether-toluene (1:4) as the mobile phase. Carol (93) separated progesterone from testosterone on a Celite column, using 80 per cent ethanol as the stationary and isoóctane as the mobile phase, and Banes (23) used the same method, but 50 per cent ethanol, for separating dianhydrogitoxigenin from digoxin.…”

“…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). Cyclohexane/formamide has also been used in the paper chromatography of corticoids (318), and cyclohexane-benzene (l:l)/formamide was used by Kochakian and Stidworthy (222) for the paper 8 The references should preferably be read in the sequences given.…”

Ab + D → Abd → Abcd

“…Other routes to estrone methyl ether include (a) isomerization of the 8-double bond to 9 (11), as in 24, and hydrogénation over palladium-oncalcium carbonate [2,4,[22][23][24][25], and (b) protection of the 17-oxo group as a cyclic ketal 25, followed by catalytic hydrogénation, lithiumammonia reduction, and hydrolysis of the ketal linkage [1,5]. Although the Torgov synthesis is usually carried out with a 3-methoxyl group, it is possible to go directly to estrone by starting with the diol 26 (R = H); condensation, cyclization, hydrogénation, isomerization, and hydrogénation steps proceed in good yield [1,2,22,[26][27][28][29][30].…”

Rapid Identification and Estimation of Gitoxin in Digitoxin and Digoxin Tablets by TLC

“…Identification Test A is a color reaction using a version of the Keller-Kiliani reagent (2). Gitoxin is the principal digitoxoside other than digitoxin occurring in digitoxin tablets (3), and separation on a diatomaceous earth1 column used in the USP XVII method is based on this premise (4). The "Other Digitoxosides" determination is also a colorimetric method based on the Keller-Kiliani reagent.…”