Emetan, 6¢,7¢,10,11-tetramethoxy-, dihydrochloride.
Emetine dihydrochloride [316-42-7].
» Emetine Hydrochloride is the hydrochloride of an alkaloid obtained from Ipecac, or prepared by methylation of cephaeline, or prepared synthetically. It contains not less than 98.0 percent and not more than 101.5 percent of C29H40N2O4·2HCl, calculated on the anhydrous basis.
Packaging and storage Preserve in tight, light-resistant containers. Store at 25, excursions permitted between 15 and 30.
B: Ultraviolet Absorption 197U
Solution: 50 µg per mL.
Medium: 0.5 N sulfuric acid.
C: A solution (1 in 20) responds to the tests for Chloride 191.
Water, Method I 921: between 15.0% and 19.0%.
Residue on ignition 281: not more than 0.2%.
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 [noteConduct this test in subdued light until after the chromatogram has been completely developed.]
Standard preparation Dissolve 23 mg of USP Cephaeline Hydrobromide RS in 100.0 mL of methanol.
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 C29H40N2O4·2HCl.
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USP32NF27 Page 2246Pharmacopeial Forum: Volume No. 29(6) Page 1875