Fluocinolone Acetonide Cream
»Fluocinolone Acetonide Cream contains not less than 90.0percent and not more than 110.0percent of the labeled amount of C24H30F2O6.
Packaging and storage— Preserve in collapsible tubes or tight containers.
Identification— Transfer a quantity of the Cream,equivalent to about 0.5mg of fluocinolone acetonide,to a centrifuge tube,disperse it in 5mLof water,add 10mLof chloroform,shake,and centrifuge.Remove and discard the aqueous layer,add 10mLof water to the tube,shake,and centrifuge.Dry about 2mLof the chloroform extract over about 200mg of anhydrous sodium sulfate:the dried extract responds to the Thin-Layer Chromatographic Identification Test á201ñ,50µLof the dried chloroform extract and 50µLof a Standard solution containing about 50µg per mLof USP Fluocinolone Acetonide RSbeing applied,and a mixture of chloroform and diethylamine (2:1)being used for development.
Microbial limits á61ñ— It meets the requirements of the tests for absence of Staphylococcus aureusand Pseudomonas aeruginosa.
Minimum fill á755ñ: meets the requirements.
Assay—
Internal standard solution— Dissolve USP Norethindrone RSin acetonitrile to obtain a solution containing about 200µg per mL.
Standard preparation— Dissolve an accurately weighed quantity of USP Fluocinolone Acetonide RSin acetonitrile to obtain a solution having a known concentration of about 300µg per mL.Transfer 5.0mLof this solution,6.0mLof Internal standard solution,and 15.0mLof water to a 50-mLvolumetric flask.Dilute with acetonitrile to volume,and mix.The Standard preparationcontains 30µg of USP Fluocinolone Acetonide RSper mL.
Mobile solvent— Prepare a mixture of water and acetonitrile (5:3).Adjust the ratio as necessary to obtain suitable chromatographic performance.
Assay preparation— Dissolve an accurately weighed portion of Cream,equivalent to about 0.75mg of fluocinolone acetonide,in about 10mLof acetonitrile by heating on a steam bath.Transfer the mixture to a 25-mLvolumetric flask with the aid of three 2-mLportions of acetonitrile.Add 3.0mLof Internal standard solutionand 5.0mLof water,cool,and mix.Dilute with acetonitrile to volume,mix,and cool in an ice bath.Centrifuge or filter the mixture to obtain a clear solution.
Apparatus— Use a high-pressure liquid chromatograph (see Chromatography á621ñ)of the general type equipped with a detector for monitoring UVabsorbance at about 254nm,and capable of providing a flow rate of about 2mLper minute for the Mobile solvent.Use a column that contains packing L1.
Procedure— Chromatograph equal volumes of the Assay preparationand the Standard preparation.Three replicate injections of the Standard preparationshow a resolution factor of not less than 2.0between the peaks for norethindrone and fluocinolone acetonide and a relative standard deviation of not more than 1.5%.Calculate the quantity,in mg,of C24H30F2O6in the portion of Cream taken by the formula:
0.025C(RU/RS),
in which Cis the concentration,in µg per mL,of USP Fluocinolone Acetonide RSin the Standard preparation;and RUand RSare the ratios of the peak areas of fluocinolone acetonide and norethindrone obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 839
Phone Number:1-301-816-8139