4H-Dibenzo[de,g]quinoline-10,11-diol, 5,6,6a,7-tetrahydro-6-methyl-, hydrochloride, hemihydrate, (R)-.
6a-Aporphine-10,11-diol hydrochloride hemihydrate [41372-20-7].
Anhydrous 303.79 [314-19-2].
» Apomorphine Hydrochloride contains not less than 98.5 percent and not more than 100.5 percent of C17H17NO2·HCl, calculated on the dried basis.
Packaging and storage Preserve in tight, light-resistant containers.
Color of solution Place 100 mg in a suitable test tube, add 10 mL of cold, oxygen-free water, and agitate gently until dissolved: the color of the resulting solution, observed promptly after the Apomorphine Hydrochloride has dissolved, is not more intense than that of a color standard prepared as follows. Dissolve 5 mg of Apomorphine Hydrochloride in 100.0 mL of water. Transfer 1.0 mL of this solution to a test tube of the same size as that used for the test solution, dilute with 6 mL of water, add 1 mL of sodium bicarbonate solution (1 in 20), and then add 0.50 mL of iodine TS. Allow to stand for 30 seconds, add 0.60 mL of sodium thiosulfate solution (1 in 40), and dilute with water to 10 mL.
B: To 5 mL of a solution (1 in 100) add a slight excess of sodium bicarbonate solution (1 in 20): a white or greenish-white precipitate is formed. Add 3 drops of iodine TS, and shake vigorously: an emerald-green color is produced. Add 5 mL of ether and, after vigorous shaking, allow the layers to separate: the ether is colored deep ruby-red while the water layer retains its green color.
C: Dissolve it in nitric acid: a dark purple solution is produced.
D: To a solution of it add silver nitrate TS: a white precipitate, which is insoluble in nitric acid, is formed. This precipitate soon darkens by reduction to metallic silver, the reduction being accelerated by the addition of 6 N ammonium hydroxide.
Specific rotation 781S: between 60.5 and 63.0.
Test solution: 15 mg per mL, in dimethylsulfoxide.
Loss on drying 731 Dry it at 105 for 2 hours: it loses between 2.0% and 3.5% of its weight.
Residue on ignition 281: not more than 0.1%.
Decomposition products Shake 100 mg with 5 mL of ether: the latter acquires not more than a pale reddish color.
Ordinary impurities 466
Solvent for Test Solution: methanol.
Solvent for Standard Solution: methanol.
Eluant: a mixture of 1-butanol, water, and formic acid (7:2:1).
Visualization: a freshly prepared mixture of 10% ferric chloride solution and 5% potassium ferricyanide solution (2:1). Allow the chromatograms to develop until the solvent front has moved about 8 cm. [noteThe development time is 1.5 to 2 hours.] Allow the plates to dry at room temperature for 1 hour prior to spraying.
Assay Dissolve about 300 mg of Apomorphine Hydrochloride, accurately weighed, in 100 mL of glacial acetic acid with the aid of heat provided by a steam bath. Add 0.1 mL of acetic anhydride to the hot solution, and stir for 5 minutes. Cool to room temperature, add 5 mL of mercuric acetate TS and 0.25 mL of crystal violet TS, and titrate with 0.1 N perchloric acid VS to a blue endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 30.38 mg of C17H17NO2·HCl.
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USP32NF27 Page 1573Pharmacopeial Forum: Volume No. 32(5) Page 1438