Packaging and storage—
Preserve in tight, light-resistant containers. Store at 25
, excursions permitted between 15
and 30
.
Acidity—
Dissolve 100 mg in 10 mL of water, add 1 drop of
methyl red TS, and titrate with 0.020 N sodium hydroxide: not more than 0.5 mL is required to produce a yellow color.
Limit of cephaeline—
[NOTE—Conduct this test in subdued light until after the chromatogram has been completely developed.
]
Test preparation—
Dissolve 100 mg of Emetine Hydrochloride in 10.0 mL of methanol.
Spray reagent—
Dissolve 300 mg of
p-nitroaniline in 25 mL of 2 N hydrochloric acid, and cool to about 4
. Slowly add 5 mL of sodium nitrite solution (1 in 25), maintaining the temperature at about 4
. Freshly prepare the solution for each test.
Procedure—
Apply 10-µL portions of the
Standard preparation and the
Test preparation, respectively, to a suitable thin-layer chromatographic plate coated with a 0.25-mm layer of chromatographic silica gel. Place the plate in a chromatographic tank containing a mixture of 9 volumes of chloroform and 1 volume of diethylamine, and develop the chromatogram until the solvent front has moved about 12 cm. Remove the plate from the tank, and allow the plate to air-dry for 20 minutes. Spray the dried plate with 2.5 N sodium hydroxide solution, and dry at 50
for 5 minutes. Then spray the plate with
Spray reagent: any cephaeline spot from the
Test preparation is not larger or more intense than that produced by the
Standard preparation (2%).
Assay—
Dissolve about 150 mg of Emetine Hydrochloride, accurately weighed, in 5 mL of glacial acetic acid, warming, if necessary. Allow the solution to cool, add 10 mL of dioxane, 5 mL of
mercuric acetate TS, and 3 drops of
crystal violet TS, and titrate with 0.1 N perchloric acid VS. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 27.68 mg of C
29H
40N
2O
4·2HCl.
;)
191
.