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.
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 (C
20H
29FO
3) in the portion of Tablets taken by the formula:
20C(RU / RS),
in which the terms are as defined therein.
