(am'' oh dye' a kwin hye'' droe klor' ide).
Phenol, 4-[(7-chloro-4-quinolinyl)amino]-2-[(diethylamino)-methyl]-, dihydrochloride, dihydrate.
4-[(7-Chloro-4-quinolyl)amino]--(diethylamino)-o-cresol dihydrochloride dihydrate [6398-98-7].
Anhydrous 428.79 [69-44-3].
» Amodiaquine Hydrochloride contains not less than 97.0 percent and not more than 103.0 percent of C20H22ClN3O·2HCl, calculated on the anhydrous basis.
Packaging and storage Preserve in tight containers.
USP Reference standards 11
Completeness of solution 641 A solution of 200 mg in 10 mL of water is clear.
A: Infrared Absorption 197KPrepare the test specimen as follows. Dissolve 20 mg in 10 mL of water in a separator, add 1 mL of ammonium hydroxide, and extract by shaking with 25 mL of chloroform. Draw off and evaporate the chloroform extract, and dry the residue at 105 for 2 hours.
B: Ultraviolet Absorption 197U
Solution: 10 µg per mL.
Medium: dilute hydrochloric acid (1 in 100).
C: A solution of it meets the requirements of the tests for Chloride 191.
D: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
Water, Method I 921: not less than 7.0% and not more than 9.0%.
Residue on ignition 281: not more than 0.2%.
Buffer, Mobile phase, Standard preparation, System suitability solution, and Chromatographic system Prepare as directed in the Assay.
Test solution Use the Assay preparation, prepared as directed in the Assay.
Procedure Proceed as directed for Procedure in the Assay. Calculate the percentage of each impurity in the portion of Amodiaquine Hydrochloride taken by the formula:
100(ri / rs)in which ri is the response of each impurity peak; and rs is the sum of the responses of all the peaks: the limit of any individual impurity peak is not more than 0.5%.
Buffer solution Accurately weigh about 13.6 g of monobasic potassium phosphate and dissolve in 2 L of water. Add 2.0 mL of perchloric acid, mix, and adjust with phosphoric acid to a pH of 2.5 ± 0.5. Pass the solution through a 0.45-µm membrane filter.
Mobile phase Prepare a mixture of Buffer solution and methanol (78:22). Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard preparation Transfer an accurately weighed quantity of USP Amodiaquine Hydrochloride RS to a suitable volumetric flask, and dissolve in and dilute with water to volume to obtain a solution having a concentration of about 0.15 mg per mL of amodiaquine hydrochloride.
Assay preparation Transfer an accurately weighed quantity of Amodiaquine Hydrochloride to a suitable volumetric flask, and dissolve in and dilute with water to volume to obtain a solution having a concentration of about 0.15 mg per mL of amodiaquine hydrochloride.
System suitability solution Transfer an accurately weighed quantity of USP Amodiaquine Hydrochloride RS and USP Chloroquine Phosphate RS to a suitable volumetric flask, and dissolve in and dilute with water to volume to obtain a solution having concentrations of about 0.15 mg per mL of amodiaquine hydrochloride and 0.15 mg per mL of chloroquine phosphate.
Chromatography system (see Chromatography 621) The liquid chromatograph is equipped with a 224-nm detector and a 4.6-mm × 10-cm column that contains 5-µm packing L1. The flow rate is about 1.2 mL per minute. The column temperature is maintained at 25 ± 5. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are 1.0 for amodiaquine hydrochloride and 0.8 for chloroquine phosphate; the resolution, R, between amodiaquine hydrochloride and chloroquine phosphate is not less than 1.5; for both compounds, the tailing factor is not more than 1.5; and the relative standard deviation is not more than 2.0%.
Procedure Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in percent, of C20H22ClN3O·2HCl in the portion of Amodiaquine Hydrochloride taken by the formula:
100(CS / CU)(rU / rS)in which 100 is the percent conversion factor; CS is the concentration, in mg per mL, of USP Amodiaquine Hydrochloride RS in the Standard preparation; CU is the concentration, in mg per mL, of Amodiaquine Hydrochloride in the Assay preparation; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 2193Pharmacopeial Forum: Volume No. 34(2) Page 243