Identification—
A:
It is soluble in 1 N potassium hydroxide or in 1 N sodium hydroxide, forming a yellow liquid, which gradually becomes darker on standing and from which the resin is precipitated by hydrochloric acid.
B:
A hot solution of it deposits most of its solids on cooling, and if the cooled liquid is filtered, the filtrate turns brown upon the addition of a few drops of
ferric chloride TS.
Hexane-insoluble matter—
Transfer about 1 g of Podophyllum Resin, accurately weighed, to a glass-stoppered, 100-mL conical flask, add 30.0 mL of chloroform, insert the stopper tightly, and shake for 30 minutes, using a mechanical wrist-action shaker, or equivalent. Filter with suction through a medium- or fine-porosity, sintered-glass filter, into a small filter flask. Wash the conical flask and the filter with two 5-mL portions of chloroform, adding the washings to the filtrate. Transfer the filtrate with the aid of chloroform to a 50-mL volumetric flask, add chloroform to volume, and mix. Pipet 20 mL of the resulting solution into a 250-mL conical flask containing 160 mL of solvent hexane. Gently swirl, allow to stand for 10 minutes, and transfer the resulting precipitate to a tared, fine-porosity, sintered-glass filter, wash the flask and the precipitate with two 20-mL portions of solvent hexane, dry the precipitate at 70
for 1 hour, and weigh the
Hexane-insoluble matter so obtained. Multiply by 2.5 to find the amount present in the quantity of Podophyllum Resin taken.
281
:
not more than 1.5%.