» Testolactone Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of C19H24O3.
Packaging and storage Preserve in tight containers.
USP Reference standards 11
A: Hydroxylamine reagentMix 5 mL of a solution of hydroxylamine hydrochloride in methanol (3.5 in 100) with 15 mL of a solution of potassium hydroxide in methanol (5.6 in 100), and use this reagent within 2 hours after mixing. [noteStore the solution of hydroxylamine hydrochloride in methanol and the solution of potassium hydroxide in methanol in a refrigerator, and discard both after 1 month. ]
Iron reagent Dissolve 1.5 g of ferric chloride in 30 mL of water, add 3 mL of perchloric acid and 15 mL of nitric acid, and heat the solution until dense, white fumes are produced. Cool, add 40 mL of water and 10 mL of nitric acid, and dilute with perchloric acid to 100 mL. [noteThis concentrate may be stored and used for several months. ] Transfer 4.0 mL of this concentrate to a 100-mL volumetric flask, add 36 mL of alcohol, dilute with water to volume, and mix.
Procedure Place a portion of finely powdered Tablets, equivalent to about 250 mg of testolactone, in a 100-mL volumetric flask, add 85 mL of chloroform, and shake by mechanical means for 30 minutes. Add chloroform to volume, mix, and centrifuge the solution. Transfer 2 mL of the supernatant to a small test tube, and evaporate with the aid of a gentle current of air to dryness. Add 0.1 mL of Hydroxylamine reagent, heat in a water bath at about 60 for 1 minute, then add 1 mL of Iron reagent: a rose-violet color is produced.
B:Infrared Absorption 197K
Test specimen Place a portion of finely powdered Tablets, equivalent to about 100 mg of testolactone, in a glass-stoppered, 35-mL centrifuge tube. Add 20 mL of chloroform, insert the stopper, and shake by mechanical means for 10 minutes. Centrifuge the mixture, and filter the supernatant into a 50-mL beaker. Evaporate on a steam bath to dryness, and dry the residue in vacuum at 100 for 3 hours.
Medium: 0.01 N hydrochloric acid; 900 mL.
Apparatus 2: 75 rpm.
Time: 120 minutes.
Procedure Determine the amount of C19H24O3 dissolved by employing UV absorption at the wavelength of maximum absorbance at about 247 nm 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 RS in 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 C19H24O3 is dissolved in 120 minutes.
Uniformity of dosage units 905: meet the requirements.
Assay preparation Weigh and finely powder not fewer than 10 Tablets. Transfer an accurately weighed portion of the powder, equivalent to about 50 mg of testolactone, to a 100-mL volumetric flask, add 85 mL of chloroform, and shake by mechanical means for 30 minutes. Add chloroform to volume, mix, and centrifuge a portion of about 10 mL of the mixture. Transfer 3.0 mL of the clear supernatant to a 50-mL volumetric flask, dilute with chloroform to volume, and mix.
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 4799Pharmacopeial Forum: Volume No. 27(6) Page 3332