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Procyclidine Hydrochloride
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C19H29NO·HCl 323.90

1-Pyrrolidinepropanol, -cyclohexyl--phenyl-, hydrochloride.
-Cyclohexyl--phenyl-1-pyrrolidinepropanol hydrochloride [1508-76-5].
» Procyclidine Hydrochloride contains not less than 99.0 percent and not more than 101.0 percent of C19H29NO·HCl, calculated on the dried basis.
Packaging and storage— Preserve in tight, light-resistant containers, and store in a dry place.
Identification—
B: Dissolve about 250 mg in 10 mL of water in a separator, render alkaline with 6 N ammonium hydroxide, and extract with three 10-mL portions of ether. Filter the ether extracts slowly through a layer of about 2 g 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 I being used (see Melting Range or Temperature 741).
C: A solution (1 in 100) responds to the tests for Chloride 191.
pH 791: between 5.0 and 6.5, in a solution (1 in 100).
Loss on drying 731— Dry it in vacuum at 105 for 4 hours: it loses not more than 0.5% of its weight.
Residue on ignition 281: not more than 0.1%.
Related compounds— Dissolve approximately 200 mg of Procyclidine Hydrochloride in 20 mL of water, and render the solution alkaline by adding 1.5 mL of 6 N ammonium hydroxide. Extract with three 15-mL portions of chloroform, wash the combined extracts with 20 mL of water, discard the water washing, and filter the chloroform solution through a layer of 3 to 4 g of anhydrous granular sodium sulfate supported on glass wool. Reduce the volume to 5 mL by evaporating with the aid of gentle heat and a current of air. Inject 2 µL of this solution into a suitable gas chromatograph (see Chromatography 621) equipped with a flame-ionization detector, and record the chromatogram to 2.5 relative 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 20,000 and 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 60 mL per 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 V 467: meets the requirements.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
Assay— Dissolve about 700 mg of Procyclidine Hydrochloride, accurately weighed, in 75 mL of glacial acetic acid in a 250-mL beaker, warming, if necessary, to effect solution. Cool, add 10 mL of mercuric acetate TS, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 32.39 mg of C19H29NO·HCl.
Auxiliary Information— Staff Liaison : Ravi Ravichandran, Ph.D., Senior Scientist
Expert Committee : (MDPP05) Monograph Development-Psychiatrics and Psychoactives
USP29–NF24 Page 1816
Phone Number : 1-301-816-8330