Fluoxymesterone Tablets
» Fluoxymesterone Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of fluoxymesterone (C20H29FO3).
Packaging and storage— Preserve in well-closed containers, protected from light.
Identification— Triturate a quantity of powdered Tablets, equivalent to about 20 mg of fluoxymesterone, with 20 mL of hot chloroform, and decant the supernatant through a filter. Repeat the extraction with two 20-mL portions of hot chloroform. Evaporate the combined chloroform solutions on a water bath to dryness, digest the residue with 5 mL of acetone, decant the supernatant, add to it 20 mL of water, and filter off the precipitate. Dissolve the precipitate in 5 mL of acetone, add 20 mL of water, and filter: the precipitate, after being dried at 105 for 3 hours, meets the requirements for Identification test A under Fluoxymesterone.
Dissolution 711
Medium: 0.01 N hydrochloric acid; 900 mL.
Apparatus 2: 75 rpm.
Time: 60 minutes.
Determine the amount of C20H29FO3 dissolved by employing the following method.
Mobile phase— Prepare a degassed and filtered solution of water and acetonitrile (58:42). Make adjustments if necessary (see Chromatography 621).
Internal standard solution— Dissolve a quantity of USP Norethindrone RS in alcohol to obtain a solution having a final concentration of about 46 µg per mL.
Standard solution— Transfer about 28 mg of USP Fluoxymesterone RS, accurately weighed, to a 25-mL volumetric flask, dissolve in and dilute with alcohol to volume, and mix. Pipet 5 mL of the resulting solution into a 250-mL volumetric flask, dilute with Dissolution Medium to volume, and mix. Pipet 5 mL of this solution and 2 mL of Internal standard solution into a 25-mL volumetric flask, dilute with Dissolution Medium to volume, and mix.
Test solution— Pipet a filtered 20-mL aliquot of the solution under test and 2 mL of Internal standard solution into a 25-mL volumetric flask, dilute with Dissolution Medium to volume, and mix.
Chromatographic system (see Chromatography 621)— The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 30-cm column that contains packing L1. The flow rate is about 3 mL per minute. Chromatograph replicate injections of the Standard solution, and measure the peak responses as directed for Procedure: the relative retention times are 0.5 for fluoxymesterone and 1.0 for norethindrone; the resolution, R, between fluoxymesterone and norethindrone is not less than 2; and the relative standard deviation is not more than 2.0%.
Procedure— Inject a volume (about 20 µL) of the Test solution into the chromatograph, record the chromatogram, and measure the responses for the major peaks. Calculate the amount of C20H29FO3 dissolved by comparison with the Standard solution, similarly chromatographed.
Tolerances— Not less than 70% (Q) of the labeled amount of C20H29FO3 is dissolved in 60 minutes.
Uniformity of dosage units 905: meet the requirements.
procedure for content uniformity—
Internal standard solution, Mobile phase, and Standard preparation— Prepare as directed in the Assay under Fluoxymesterone.
Test preparation— Transfer 1 Tablet to a suitable container, add 2 mL of water, and sonicate for 30 minutes or until the Tablet completely disintegrates. Add an accurately measured volume of Internal standard solution (5.0 mL for each mg of fluoxymesterone in the Tablet), and shake the mixture for 15 minutes. Filter a portion of the chloroform layer, and use the clear filtrate.
Procedure— Proceed as directed in the Assay under Fluoxymesterone, using the Test preparation in place of the Assay preparation. Calculate the quantity, in mg, of fluoxymesterone (C20H29FO3) in the Tablet taken by the formula:
(TC/D)(RU / RS)
in which T is the labeled quantity, in mg, of fluoxymesterone in the Tablet; D is the concentration, in mg per mL, of fluoxymesterone in the Test preparation, based on the labeled quantity per Tablet and the extent of dilution; and the other terms are as defined therein.
Assay—
Internal standard solution, Mobile phase, and Standard preparation— Prepare as directed in the Assay under Fluoxymesterone.
Assay preparation— Accurately weigh 20 Tablets, and grind to a fine powder in a mortar and pestle. Accurately weigh a portion of the powder, equivalent to about 5 mg of fluoxymesterone, and transfer to a suitable container. Add 20.0 mL of Internal standard solution, sonicate for 10 minutes, and shake for 15 minutes. Filter a portion of the liquid, and analyze the clear filtrate as directed for Procedure.
Procedure— Proceed as directed in the Assay under Fluoxymesterone. Calculate the quantity, in mg, of fluoxymesterone (C20H29FO3) in the portion of Tablets taken by the formula:
20C(RU / RS)
in which the terms are as defined therein.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Daniel K. Bempong, Ph.D.
Senior Scientist
1-301-816-8143
(MDPS05) Monograph Development-Pulmonary and Steroids
Reference Standards Lili Wang, Technical Services Scientist
1-301-816-8129
RSTech@usp.org
711 Margareth R.C. Marques, Ph.D.
Senior Scientist
1-301-816-8106
(BPC05) Biopharmaceutics05
USP32–NF27 Page 2420
Pharmacopeial Forum: Volume No. 30(1) Page 105
Chromatographic Column—
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.