Azatadine Maleate Tablets
»Azatadine Maleate Tablets contain not less than 90.0percent and not more than 110.0percent of the labeled amount of C20H22N2·2C4H4O4.
Packaging and storage— Preserve in well-closed containers.
Identification— Transfer 15.0mLof the Standard preparationand 15.0mLof the Assay preparation,respectively,prepared as directed in the Assay,to separate 50-mLcentrifuge tubes fitted with glass stoppers.To each centrifuge tube add 10.0mLof 1.0Nsodium hydroxide and 20mLof solvent hexane,insert the stoppers,rotate the centrifuge tubes for about 15minutes,and centrifuge.Transfer the solvent hexane extracts (upper phase)from each centrifuge tube to separate 50-mLconical flasks fitted with glass stoppers.Evaporate the solvent hexane extracts on a steam bath under a stream of nitrogen to dryness,pipet 1mLof 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 100µLeach of the test solution and the Standard solution to a suitable thin-layer chromatographic plate (see Chromatography á621ñ)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 UVlight:the RFvalue and intensity of the principal spot in the chromatogram of the test solution correspond to those obtained from the chromatogram of the Standard solution.
Dissolution á711ñ—
Medium: 0.01Nhydrochloric acid;500mL.
Apparatus 2: 50rpm.
Time: 30minutes.
Procedure— Determine the amount of C20H22N2·2C4H4O4dissolved by employing UVabsorption at the wavelength of maximum absorbance at about 283nm 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 RSin the same Medium.
Tolerances— Not less than 80%(Q)of the labeled amount of C20H22N2·2C4H4O4is dissolved in 30minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Assay—
Standard preparation— Dissolve an accurately weighed quantity of USP Azatadine Maleate RSin 0.1Nhydrochloric acid,and dilute quantitatively,and stepwise if necessary,with 0.1Nhydrochloric acid to obtain a solution having a known concentration of about 0.06mg per mL.
Assay preparation— Weigh and finely powder not fewer than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 1.5mg of azatadine maleate,to a 50-mLflask fitted with a glass stopper.Add 25.0mLof 0.1Nhydrochloric acid,insert the stopper,and shake the mixture by mechanical means for about 30minutes.Filter the mixture into a suitable glass-stoppered vessel,discarding the first 5mLof the filtrate.
Procedure— Separately transfer 15.0mLof the Standard preparation,15.0mLof the Assay preparation,and 15.0mLof 0.1Nhydrochloric acid to provide the reagent blank to three 50-mLcentrifuge tubes fitted with glass stoppers.To each centrifuge tube add 10.0mLof 1.0Nsodium hydroxide and 20mLof solvent hexane,insert the stoppers,rotate the centrifuge tubes for about 15minutes,and centrifuge until the supernatants (solvent hexane phase)are clear.With the aid of separate syringes,transfer the supernatants to separate 50-mLcentrifuge tubes fitted with glass stoppers.Rinse each syringe with 10mLof 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 10minutes,and centrifuge.Transfer each supernatant to the respective supernatant previously collected.Pipet 15mLof 0.1Nhydrochloric acid into each centrifuge tube containing the combined supernatants,insert the stoppers,rotate each tube for about 15minutes,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 283nm,with a suitable spectrophotometer zeroed with 0.1Nhydrochloric acid,using the prepared reagent blank.Calculate the quantity,in mg,of C20H22N2·2C4H4O4in the portion of Tablets taken by the formula:
25C(AU/AS),
in which Cis the concentration,in mg per mL,of USP Azatadine Maleate RSin the Standard preparation;and AUand ASare the absorbances of the solutions from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Karen A Russo,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 206
Phone Number:1-301-816-8379
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