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1,4-Benzenediamine, 2,6-dichloro-N1-2-imidazolidinylidene-, monohydrochloride.
2-[(4-Amino-2,6-dichlorophenyl)imino]imidazolidine monohydrochloride [73218-79-8].
» Apraclonidine Hydrochloride contains not less than 98.0 percent and not more than 102.0 percent of C9H10Cl2N4·HCl, calculated on the dried basis.
Packaging and storage Preserve in tight, light-resistant containers.
USP Reference standards 11
pH 791: between 5.0 and 6.6 in a solution (1 in 100).
Loss on drying 731 Dry it in vacuum at 105 for 3 hours: it loses not more than 1.0% of its weight.
Residue on ignition 281: not more than 0.1%.
Heavy metals, Method II 231: 0.002%.
Phosphate buffer Transfer 6.8 mL of phosphoric acid to a 2000-mL volumetric flask, add about 1900 mL of water, and mix. Adjust with sodium hydroxide solution (1 in 2) to a pH of 3.0, dilute with water to volume, and mix.
Mobile phase Prepare a filtered and degassed mixture of acetonitrile, Phosphate buffer, and methanol (56:40:4). Make adjustments if necessary (see System Suitability under Chromatography 621).
System suitability solution Prepare a solution in Mobile phase containing about 0.8 mg of USP Apraclonidine Hydrochloride RS per mL.
Test solution Transfer about 20 mg of Apraclonidine Hydrochloride, accurately weighed, to a 25-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)The liquid chromatograph is equipped with a 220-nm detector and an 8-mm × 100-mm column that contains packing L7. The flow rate is about 3 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the tailing factor for the apraclonidine peak is not more than 2.2, and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure Inject about 20 µL of the Test solution into the chromatograph, record the chromatogram, and measure the areas for the major peaks. [noteAllow about five times the elution time of apraclonidine before making the next injection. ] Calculate the percentage of each peak, other than the solvent peak and the apraclonidine peak, in the specimen of Apraclonidine Hydrochloride taken by the same formula:
100ri / rtin which ri is the response of each peak other than the principal peak, and rt is the sum of the responses of all of the peaks, excluding that of the solvent peak: not more than 1.0% for any individual impurity and not more than 2.0% total impurities are found.
Assay Dissolve about 125 mg of Apraclonidine Hydrochloride, accurately weighed, in 40 mL of glacial acetic acid. Add 10 mL of mercuric acetate TS, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically from the second inflection point, using a calomel-glass electrode system (see Titrimetry 541). Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 14.08 mg of C9H10Cl2N4·HCl.
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USP35NF30 Page 2234