Testolactone Tablets
»Testolactone Tablets contain not less than 90.0percent and not more than 110.0percent of the labeled amount of C19H24O3.
Packaging and storage— Preserve in tight containers.
Identification—
A: Hydroxylamine reagent—Mix 5mLof a solution of hydroxylamine hydrochloride in methanol (3.5in 100)with 15mLof a solution of potassium hydroxide in methanol (5.6in 100),and use this reagent within 2hours after mixing.[NOTE—Store the solution of hydroxylamine hydrochloride in methanol and the solution of potassium hydroxide in methanol in a refrigerator,and discard both after 1month.]
Iron reagent— Dissolve 1.5g of ferric chloride in 30mLof water,add 3mLof perchloric acid and 15mLof nitric acid,and heat the solution until dense,white fumes are produced.Cool,add 40mLof water and 10mLof nitric acid,and dilute with perchloric acid to 100mL.[NOTE—This concentrate may be stored and used for several months.]Transfer 4.0mLof this concentrate to a 100-mLvolumetric flask,add 36mLof alcohol,dilute with water to volume,and mix.
Procedure— Place a portion of finely powdered Tablets,equivalent to about 250mg of testolactone,in a 100-mLvolumetric flask,add 85mLof chloroform,and shake by mechanical means for 30minutes.Add chloroform to volume,mix,and centrifuge the solution.Transfer 2mLof the supernatant to a small test tube,and evaporate with the aid of a gentle current of air to dryness.Add 0.1mLofHydroxylamine reagent,heat in a water bath at about 60for 1minute,then add 1mLofIron reagent:a rose-violet color is produced.
B:Infrared Absorption á197Kñ—
Test specimen— Place a portion of finely powdered Tablets,equivalent to about 100mg of testolactone,in a glass-stoppered,35-mLcentrifuge tube.Add 20mLof chloroform,insert the stopper,and shake by mechanical means for 10minutes.Centrifuge the mixture,and filter the supernatant into a 50-mLbeaker.Evaporate on a steam bath to dryness,and dry the residue in vacuum at 100for 3hours.
Dissolution á711ñ—
Medium: 0.01Nhydrochloric acid;900mL.
Apparatus 2: 75rpm.
Time: 120minutes.
Procedure— Determine the amount of C19H24O3dissolved by employing UVabsorption at the wavelength of maximum absorbance at about 247nm on filtered portions of the solution under test,diluted with water if necessary,in comparison with a Standard solution having a known concentration of USP Testolactone RSin the same medium.An amount of methanol not to exceed 2%of the total volume of the Standard solution may be used to bring the testolactone standard into solution prior to dilution with water.
Tolerances— Not less than 80%(Q)of the labeled amount of C19H24O3is dissolved in 120minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Assay—
Isoniazid reagentand Standard preparation— Prepare as directed in theAssayunderTestolactone.
Assay preparation— Weigh and finely powder not fewer than 10Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 50mg of testolactone,to a 100-mLvolumetric flask,add 85mLof chloroform,and shake by mechanical means for 30minutes.Add chloroform to volume,mix,and centrifuge a portion of about 10mLof the mixture.Transfer 3.0mLof the clear supernatant to a 50-mLvolumetric flask,dilute with chloroform to volume,and mix.
Procedure— Proceed as directed forProcedurein theAssayunderTestolactone.Calculate the quantity,in mg,of C19H24O3in the portion of Tablets taken by the formula:
1.667C(AU/AS),
in which the terms are as defined therein.
Auxiliary Information— Staff Liaison:Lawrence Evans,III,Ph.D.,Scientist
Expert Committee:(PA6)Pharmaceutical Analysis 6
USP28–NF23Page 1875
Pharmacopeial Forum:Volume No.27(6)Page 3332
Phone Number:1-301-816-8389