Danazol
;)
Pregna-2,4-dien-20-yno[2,3-d]isoxazol-17-ol,(17a)-.
17a-Pregna-2,4-dien-20-yno[2,3-d]isoxazol-17-ol [17230-88-5].
»Danazol contains not less than 97.0percent and not more than 102.0percent of C22H27NO2,calculated on the dried basis.
Packaging and storage—
Preserve in tight,light-resistant containers.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Ultraviolet Absorption á197Uñ—
Solution:
prepared as directed in theAssay.
Specific rotation á781Sñ:
between +21
and +27.
and +27.
Test solution:
10mg per mL,in chloroform.
Loss on drying á731ñ—
Dry it at a pressure not exceeding 5mm of mercury at 60to constant weight:it loses not more than 2.0%of its weight.
to constant weight:it loses not more than 2.0%of its weight.
Chromatographic purity—
Solvent—
Prepare a mixture of chloroform and methanol (9:1).
Standard solutions—
Dissolve an accurately weighed quantity of USP Danazol RSinSolventto obtain a solution having a known concentration of 1mg per mL.Dilute quantitatively withSolventto obtain Standard solutionshaving the following compositions:
| Standard
solution |
Dilution | Concentration (µg RSper mL) |
Percentage (%, for comparison with test specimen) |
| A | (1in 2) | 500 | 1.0 |
| B | (1in 4) | 250 | 0.5 |
| C | (1in 10) | 100 | 0.2 |
| D | (1in 20) | 50 | 0.1 |
Test solution—
Dissolve an accurately weighed quantity of Danazol inSolventto obtain a solution containing 50mg per mL.
Procedure—
Apply separately 5µLof theTest solutionand 5µLof eachStandard solutionto a suitable thin-layer chromatographic plate (seeChromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture.Position the plate in a chromatographic chamber and develop the chromatograms in a solvent system consisting of a mixture of cyclohexane and ethyl acetate (7:3)until the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the developing chamber,mark the solvent front,and allow the solvent to evaporate in warm,circulating air.Examine the plate under short-wavelength UVlight.Expose the plate to iodine vapors for 5minutes.Compare the intensities of any secondary spots observed in the chromatogram of theTest solution with those of the principal spots in the chromatograms of theStandard solutions:the sum of the intensities of secondary spots obtained from theTest solutioncorresponds to not more than 1.0%of related compounds,with no single impurity corresponding to more than 0.5%.
Organic volatile impurities,Method IVá467ñ:
meets the requirements.
Assay—
Dissolve about 100mg of Danazol,accurately weighed and previously dried,in about 50mLof alcohol in a 100-mLvolumetric flask,swirl until dissolved,dilute with alcohol to volume,and mix.Transfer 2.0mLof this solution to a 100-mLvolumetric flask,dilute with alcohol to volume,and mix.Similarly,dissolve an accurately weighed quantity of USP Danazol RSin alcohol to obtain a Standard solution having a known concentration of about 20µg per mL.Concomitantly determine the absorbances of both solutions in 1-cm cells at the wavelength of maximum absorbance at about 285nm,using alcohol as the blank.Calculate the quantity,in mg,of C22H27NO2in the portion of Danazol taken by the formula:
5C(AU/AS),
in whichCis the concentration,in µg per mL,of USP Danazol RSin the Standard solution;and AUand ASare the absorbances of the solution of Danazol and the Standard solution,respectively.
Auxiliary Information—
Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 571
Pharmacopeial Forum:Volume No.27(6)Page 3269
Phone Number:1-301-816-8139