Azatadine Maleate Tablets
» Azatadine Maleate Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of C20H22N2·2C4H4O4.
Packaging and storage Preserve in well-closed containers.
Identification Transfer 15.0 mL of the Standard preparation and 15.0 mL of the Assay preparation, respectively, prepared as directed in the Assay, to separate 50-mL centrifuge tubes fitted with glass stoppers. To each centrifuge tube add 10.0 mL of 1.0 N sodium hydroxide and 20 mL of solvent hexane, insert the stoppers, rotate the centrifuge tubes for about 15 minutes, and centrifuge. Transfer the solvent hexane extracts (upper phase) from each centrifuge tube to separate 50-mL conical flasks fitted with glass stoppers. Evaporate the solvent hexane extracts on a steam bath under a stream of nitrogen to dryness, pipet 1 mL of solvent hexane into each flask, insert the stoppers, and mix by use of a vortex mixer (or equivalent) until the residues have dissolved. Use these solutions as the Standard solution and the test solution, respectively. Apply separately 100 µL each of the test solution and the Standard solution to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic silica gel mixture. Allow the spots to dry, and develop the chromatogram in a solvent system consisting of toluene, isopropyl alcohol, and diethylamine (10:10:1) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the plate to air-dry. Examine the plate under short-wavelength UV light: the RF value and intensity of the principal spot in the chromatogram of the test solution correspond to those obtained from the chromatogram of the Standard solution.
Medium: 0.01 N hydrochloric acid; 500 mL.
Apparatus 2: 50 rpm.
Time: 30 minutes.
Procedure Determine the amount of C20H22N2·2C4H4O4 dissolved by employing UV absorption at the wavelength of maximum absorbance at about 283 nm on filtered portions of the solution under test, diluted with Medium, if necessary, in comparison with a Standard solution having a known concentration of USP Azatadine Maleate RS in the same Medium.
Tolerances Not less than 80% (Q) of the labeled amount of C20H22N2·2C4H4O4 is dissolved in 30 minutes.
Uniformity of dosage units 905: meet the requirements.
Standard preparation Dissolve an accurately weighed quantity of USP Azatadine Maleate RS in 0.1 N hydrochloric acid, and dilute quantitatively, and stepwise if necessary, with 0.1 N hydrochloric acid to obtain a solution having a known concentration of about 0.06 mg per mL.
Assay preparation Weigh and finely powder not fewer than 20 Tablets. Transfer an accurately weighed portion of the powder, equivalent to about 1.5 mg of azatadine maleate, to a 50-mL flask fitted with a glass stopper. Add 25.0 mL of 0.1 N hydrochloric acid, insert the stopper, and shake the mixture by mechanical means for about 30 minutes. Filter the mixture into a suitable glass-stoppered vessel, discarding the first 5 mL of the filtrate.
Procedure Separately transfer 15.0 mL of the Standard preparation, 15.0 mL of the Assay preparation, and 15.0 mL of 0.1 N hydrochloric acid to provide the reagent blank to three 50-mL centrifuge tubes fitted with glass stoppers. To each centrifuge tube add 10.0 mL of 1.0 N sodium hydroxide and 20 mL of solvent hexane, insert the stoppers, rotate the centrifuge tubes for about 15 minutes, and centrifuge until the supernatants (solvent hexane phase) are clear. With the aid of separate syringes, transfer the supernatants to separate 50-mL centrifuge tubes fitted with glass stoppers. Rinse each syringe with 10 mL of solvent hexane, and add the rinse to the aqueous phase from which the respective supernatant was removed. Insert the stoppers, rotate each tube for about 10 minutes, and centrifuge. Transfer each supernatant to the respective supernatant previously collected. Pipet 15 mL of 0.1 N hydrochloric acid into each centrifuge tube containing the combined supernatants, insert the stoppers, rotate each tube for about 15 minutes, and centrifuge. Remove and discard the supernatants. Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance at about 283 nm, with a suitable spectrophotometer zeroed with 0.1 N hydrochloric acid, using the prepared reagent blank. Calculate the quantity, in mg, of C20H22N2·2C4H4O4 in the portion of Tablets taken by the formula:
25C(AU / AS)in which C is the concentration, in mg per mL, of USP Azatadine Maleate RS in the Standard preparation; and AU and AS are the absorbances of the solutions from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP32NF27 Page 1610