Anileridine Hydrochloride
C22H28N2O2·2HCl
425.39
4-Piperidinecarboxylic acid,1-[2-(4-aminophenyl)ethyl]-4-phenyl-,ethyl ester,dihydrochloride.
Ethyl 1-(p-aminophenethyl)-4-phenylisonipecotate dihydrochloride [126-12-5].
»Anileridine Hydrochloride contains not less than 96.0percent and not more than 102.0percent of C22H28N2O2·2HCl,calculated on the dried basis.
Packaging and storage—
Preserve in tight,light-resistant containers.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Dissolve 50mg in water in a 100-mLvolumetric flask,dilute with water to volume,and mix (Stock solution).Transfer 4.0mLof this solution to a 100-mLvolumetric flask,and add 25mLof pH7.0Buffer solution.(Prepare the pH7.0Buffer solutionby dissolving 22.73g of anhydrous dibasic sodium phosphate and 14.52g of monobasic potassium phosphate in water to make 1000.0mL.Dilute 25mLof the buffer with water to 100mL:the pH,determined potentiometrically,is 7.0±0.05.)Dilute with water to volume,and mix (Solution A).Transfer 20.0mLof the Stock solutionto a 100-mLvolumetric flask,add 25mLof the pH7.0Buffer solution,dilute with water to volume,and mix (Solution B):the UVabsorption spectrum of Solution Aexhibits a maximum at 234±1nm,and the UVabsorption spectrum of Solution Bexhibits a maximum at 285±2nm.
C:
To 5mLof a solution (1in 5000)add 2mLof a 1in 100solution of p-dimethylaminobenzaldehyde in alcohol:a yellow color develops immediately.
D:
Asolution (1in 100)responds to the tests for Chloride á191ñ.
pHá791ñ:
between 2.5and 3.0,in a solution (1in 20).
Loss on drying á731ñ—
Dry it at a pressure below 5mm of mercury at 100
for 2hours:it loses not more than 1.0%of its weight.
for 2hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ:
not more than 0.1%.
Chloride content—
Dissolve about 200mg,accurately weighed,in 50mLof water in a glass-stoppered flask.Add 25.0mLof 0.1Nsilver nitrate VS,then add 5mLof 2Nnitric acid and 5mLof nitrobenzene,shake vigorously,add 2mLof ferric ammonium sulfate TS,and titrate the excess silver nitrate with 0.1Nammonium thiocyanate VS.Each mLof 0.1Nsilver nitrate is equivalent to 3.545mg of Cl:the content of Cl is between 16.0%and 17.2%.
Assay—
Dissolve about 200mg of Anileridine Hydrochloride,accurately weighed,in 10mLof glacial acetic acid by heating on a steam bath.Cool immediately in a cold water bath,add 5mLof mercuric acetate TS,20mLof acetone,and 0.5mLof indicator solution (70mg of a-naphtholbenzein,10mg of crystal violet,and 40mg of quinaldine red in 100mLof glacial acetic acid),and titrate with 0.1Nperchloric acid VSto a gray-green endpoint.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 21.27mg of C22H28N2O2·2HCl.
Auxiliary Information—
Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA2)Pharmaceutical Analysis 2
USP28–NF23Page 160
Phone Number:1-301-816-8139