Emetine Hydrochloride
;)
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 98.0percent and not more than 101.5percent of C29H40N2O4·2HCl,calculated on the anhydrous basis.
Packaging and storage—
Preserve in tight,light-resistant containers.Store at 25
,excursions permitted between 15and 30.
,excursions permitted between 15and 30.
Identification—
A:Infrared Absorption á197Kñ.
C:
Asolution (1in 20)responds to the tests for Chloride á191ñ.
Water,Method Iá921ñ:
between 15.0%and 19.0%.
Residue on ignition á281ñ:
not more than 0.2%.
Acidity—
Dissolve 100mg in 10mLof water,add 1drop of methyl red TS,and titrate with 0.020Nsodium hydroxide:not more than 0.5mLis required to produce a yellow color.
Limit of cephaeline—
[NOTE—Conduct this test in subdued light until after the chromatogram has been completely developed.]
Standard preparation—
Dissolve 23mg of USP Cephaeline Hydrobromide RSin 100.0mLof methanol.
Test preparation—
Dissolve 100mg of Emetine Hydrochloride in 10.0mLof methanol.
Spray reagent—
Dissolve 300mg of p-nitroaniline in 25mLof 2Nhydrochloric acid,and cool to about 4.Slowly add 5mLof sodium nitrite solution (1in 25),maintaining the temperature at about 4.Freshly prepare the solution for each test.
.Slowly add 5mLof sodium nitrite solution (1in 25),maintaining the temperature at about 4.Freshly prepare the solution for each test.
Procedure—
Apply 10-µLportions of the Standard preparationand 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 9volumes of chloroform and 1volume of diethylamine,and develop the chromatogram until the solvent front has moved about 12cm.Remove the plate from the tank,and allow the plate to air-dry for 20minutes.Spray the dried plate with 2.5Nsodium hydroxide solution,and dry at 50for 5minutes.Then spray the plate with Spray reagent:any cephaeline spot from the Test preparationis not larger or more intense than that produced by the Standard preparation(2%).
for 5minutes.Then spray the plate with Spray reagent:any cephaeline spot from the Test preparationis not larger or more intense than that produced by the Standard preparation(2%).
Assay—
Dissolve about 150mg of Emetine Hydrochloride,accurately weighed,in 5mLof glacial acetic acid,warming,if necessary.Allow the solution to cool,add 10mLof dioxane,5mLof mercuric acetate TS,and 3drops of crystal violet TS,and titrate with 0.1Nperchloric acid VS.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 27.68mg of C29H40N2O4·2HCl.
Auxiliary Information—
Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 729
Pharmacopeial Forum:Volume No.29(6)Page 1875
Phone Number:1-301-816-8394