Fluoxymesterone Tablets
»Fluoxymesterone Tablets contain not less than 90.0percent and not more than 110.0percent 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 20mg of fluoxymesterone,with 20mLof hot chloroform,and decant the supernatant through a filter.Repeat the extraction with two 20-mLportions of hot chloroform.Evaporate the combined chloroform solutions on a water bath to dryness,digest the residue with 5mLof acetone,decant the supernatant,add to it 20mLof water,and filter off the precipitate.Dissolve the precipitate in 5mLof acetone,add 20mLof water,and filter:the precipitate,after being dried at 105for 3hours,meets the requirements for Identificationtest Aunder Fluoxymesterone.
Change to read:
Dissolution á711ñ—
Medium: 0.01Nhydrochloric acid;900mL.
Apparatus 2: 75rpm.
Time: 60minutes.
Determine the amount of C20H29FO3dissolved 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 á621ñ).
Internal standard solution— Dissolve a quantity of USP Norethindrone RSUSP28in alcohol to obtain a solution having a final concentration of about 46µg per mL.
Standard solution— Transfer about 28mg of USP Fluoxymesterone RS,accurately weighed,to a 25-mLvolumetric flask,dissolve in and dilute with alcohol to volume,and mix.Pipet 5mLof the resulting solution into a 250-mLvolumetric flask,dilute with Dissolution Mediumto volume,and mix.Pipet 5mLof this solution and 2mLof Internal standard solutioninto a 25-mLvolumetric flask,dilute with Dissolution Mediumto volume,and mix.
Test solution— Pipet a filtered 20-mLaliquot of the solution under test and 2mLof Internal standard solutioninto a 25-mLvolumetric flask,dilute with Dissolution Mediumto volume,and mix.
Chromatographic system(see Chromatography á621ñ)— 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 3mLper minute.Chromatograph replicate injections of the Standard solution,and measure the peak responses as directed for Procedure:the relative retention times are 0.5for fluoxymesterone and 1.0for 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 20µL)of the Test solutioninto the chromatograph,record the chromatogram,and measure the responses for the major peaks.Calculate the amount of C20H29FO3dissolved by comparison with the Standard solution,similarly chromatographed.
Tolerances— Not less than 70%(Q)of the labeled amount of C20H29FO3is dissolved in 60minutes.
Uniformity of dosage units á905ñ: meet the requirements.
PROCEDURE FOR CONTENT UNIFORMITY—
Internal standard solution,Mobile phase,and Standard preparation— Prepare as directed in the Assayunder Fluoxymesterone.
Test preparation— Transfer 1Tablet to a suitable container,add 2mLof water,and sonicate for 30minutes or until the Tablet completely disintegrates.Add an accurately measured volume of Internal standard solution(5.0mLfor each mg of fluoxymesterone in the Tablet),and shake the mixture for 15minutes.Filter a portion of the chloroform layer,and use the clear filtrate.
Procedure— Proceed as directed in the Assayunder Fluoxymesterone,using the Test preparationin 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 Tis the labeled quantity,in mg,of fluoxymesterone in the Tablet;Dis 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 Assayunder Fluoxymesterone.
Assay preparation— Accurately weigh 20Tablets,and grind to a fine powder in a mortar and pestle.Accurately weigh a portion of the powder,equivalent to about 5mg of fluoxymesterone,and transfer to a suitable container.Add 20.0mLof Internal standard solution,sonicate for 10minutes,and shake for 15minutes.Filter a portion of the liquid,and analyze the clear filtrate as directed for Procedure.
Procedure— Proceed as directed in the Assayunder 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— Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 857
Pharmacopeial Forum:Volume No.30(1)Page 105
Phone Number:1-301-816-8139