Procyclidine Hydrochloride
;)
1-Pyrrolidinepropanol,a-cyclohexyl-a-phenyl-,hydrochloride.
a-Cyclohexyl-a-phenyl-1-pyrrolidinepropanol hydrochloride [1508-76-5].
»Procyclidine Hydrochloride contains not less than 99.0percent and not more than 101.0percent of C19H29NO·HCl,calculated on the dried basis.
Packaging and storage—
Preserve in tight,light-resistant containers,and store in a dry place.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Dissolve about 250mg in 10mLof water in a separator,render alkaline with 6Nammonium hydroxide,and extract with three 10-mLportions of ether.Filter the ether extracts slowly through a layer of about 2g of anhydrous granular sodium sulfate supported on glass wool,evaporate the ether with a current of warm air,and scratch the surface of the container to induce crystallization of the residue:the procyclidine so obtained melts between 83
and 87,the procedure for Class Ibeing used (see Melting Range or Temperature á741ñ).
and 87,the procedure for Class Ibeing used (see Melting Range or Temperature á741ñ).
C:
Asolution (1in 100)responds to the tests for Chloride á191ñ.
pHá791ñ:
between 5.0and 6.5,in a solution (1in 100).
Loss on drying á731ñ—
Dry it in vacuum at 105for 4hours:it loses not more than 0.5%of its weight.
for 4hours:it loses not more than 0.5%of its weight.
Residue on ignition á281ñ:
not more than 0.1%.
Related compounds—
Dissolve approximately 200mg of Procyclidine Hydrochloride in 20mLof water,and render the solution alkaline by adding 1.5mLof 6Nammonium hydroxide.Extract with three 15-mLportions of chloroform,wash the combined extracts with 20mLof water,discard the water washing,and filter the chloroform solution through a layer of 3to 4g of anhydrous granular sodium sulfate supported on glass wool.Reduce the volume to 5mLby evaporating with the aid of gentle heat and a current of air.Inject 2µLof this solution into a suitable gas chromatograph (see Chromatography á621ñ)equipped with a flame-ionization detector,and record the chromatogram to 2.5relative to the retention time of the principal (procyclidine)peak.Under typical conditions,the instrument contains a 1-m ×2-mm glass column packed with 10%polyethylene glycol 20,000and 2%potassium hydroxide on packing S1A.The column is maintained at a temperature of about 180,the injection port is maintained at 210,the detector block is maintained at about 220,and dry helium is used as the carrier gas at a flow rate of about 60mLper minute.From the total area under the curve,excluding the solvent peak,calculate the percentage of total impurities by area normalization:not more than 4.0%is found.
,the injection port is maintained at 210,the detector block is maintained at about 220,and dry helium is used as the carrier gas at a flow rate of about 60mLper minute.From the total area under the curve,excluding the solvent peak,calculate the percentage of total impurities by area normalization:not more than 4.0%is found.
Organic volatile impurities,Method Vá467ñ:
meets the requirements.
Assay—
Dissolve about 700mg of Procyclidine Hydrochloride,accurately weighed,in 75mLof glacial acetic acid in a 250-mLbeaker,warming,if necessary,to effect solution.Cool,add 10mLof mercuric acetate TS,and titrate with 0.1Nperchloric acid VS,determining the endpoint potentiometrically.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 32.39mg of C19H29NO·HCl.
Auxiliary Information—
Staff Liaison:Salvador C.Salado,M.S.,Scientist and Latin American Liaison
Expert Committee:(PA3)Pharmaceutical Analysis 3
USP28–NF23Page 1634
Phone Number:1-301-816-8165