Oxymetholone Tablets
»Oxymetholone Tablets contain not less than 90.0percent and not more than 110.0percent of the labeled amount of C21H32O3.
Packaging and storage— Preserve in well-closed containers.
Identification— Mix an amount of powdered Tablets,equivalent to about 50mg of oxymetholone,with 15mLof solvent hexane,and stir occasionally for 15minutes.Centrifuge the mixture,and decant and discard the solvent hexane.Extract the residue with two 10-mLportions of solvent hexane,centrifuging and decanting as before,and discard the solvent hexane.Add 25mLof chloroform to the residue,mix by shaking for 1to 2minutes,and filter.Evaporate the filtrate to about 3mL,add a few mLof solvent hexane to induce crystallization,and evaporate to dryness:the IRabsorption spectrum of a potassium bromide dispersion prepared from the oxymetholone so obtained,and previously dried,exhibits maxima only at the same wavelengths as that of a similar preparation of USP Oxymetholone RS,crystallized from the same solvent mixture.
Dissolution á711ñ—
Medium: 0.05MpH8.5alkaline borate buffer (see under Solutionsin the section Reagents,Indicators,and Solutions);900mL.
Apparatus 1: 100rpm.
Time: 45minutes.
Procedure— Determine the amount of C21H32O3dissolved from UVabsorbances at the wavelength of maximum absorbance at about 313nm of filtered portions of the solution under test,suitably diluted with Dissolution Mediumif necessary,in comparison with a Standard solution having a known concentration of USP Oxymetholone RSin the same medium.[NOTE—An amount of acetonitrile not to exceed 5%of the total volume of the Standard solution may be used to bring the Reference Standard into solution prior to dilution with Dissolution Medium.]
Tolerances— Not less than 75%(Q)of the labeled amount of C21H32O3is dissolved in 45minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Procedure for content uniformity— Transfer 1finely powdered Tablet to a 100-mLvolumetric flask with the aid of about 75mLof methanol.Heat the methanol to boiling,and allow to remain at a temperature just below the boiling point for 15minutes with occasional swirling.Cool to room temperature,dilute with methanol to volume,and mix.Centrifuge a portion of the mixture at about 2000rpm until the solution becomes clear.Transfer a portion of the supernatant,equivalent to about 1mg of oxymetholone,to a 100-mLvolumetric flask.Add 10mLof a 1in 250solution of sodium hydroxide in methanol,and dilute with methanol to volume.Without delay,concomitantly determine the absorbances of this solution and a freshly prepared Standard solution of USP Oxymetholone RSin the same medium having a known concentration of about 10µg per mLin 1-cm cells at the wavelength of maximum absorbance at about 315nm,with a suitable spectrophotometer,using a 1in 2500solution of sodium hydroxide in methanol as the blank.Calculate the quantity,in mg,of C21H32O3in the Tablet taken by the formula:
(TC/D)(AU/AS),
in which Tis the labeled quantity,in mg,of oxymetholone in the Tablet,Cis the concentration,in µg per mL,of USP Oxymetholone RSin the Standard solution,Dis the concentration,in µg per mL,of oxymetholone in the solution from the Tablet,based upon the labeled quantity per Tablet and the extent of dilution,and AUand ASare the absorbances of the solution from the Tablet and the Standard solution,respectively.
Assay— Weigh and finely powder not less than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 20mg of oxymetholone,to a separator,add 10mLof water,and extract with three 25-mLportions of chloroform,filtering each extract through chloroform-washed cotton.Evaporate the combined chloroform extracts on a steam bath to dryness,reducing the application of heat as dryness is approached.Dissolve the residue in methanol,transfer to a 100-mLvolumetric flask,dilute with methanol to volume,and mix.Transfer 5.0mLof the solution to a 100-mLvolumetric flask,add 10mLof a 1in 250solution of sodium hydroxide in methanol,dilute with methanol to volume,and mix.Without delay,concomitantly determine the absorbances of this solution and a freshly prepared Standard solution of USP Oxymetholone RSin the same medium having a known concentration of about 10µg per mLin 1-cm cells at the wavelength of maximum absorbance at about 315nm,with a suitable spectrophotometer,using a 1in 2500solution of sodium hydroxide in methanol as the blank.Calculate the quantity,in mg,of C21H32O3in the portion of Tablets taken by the formula:
2C(AU/AS),
in which Cis the concentration,in µg per mL,of USP Oxymetholone RSin the Standard solution,and AUand ASare the absorbances of the solution from the Tablets and the Standard solution,respectively.
Auxiliary Information— Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1445
Phone Number:1-301-816-8139