Oxandrolone
;)
2-Oxaandrostan-3-one,17-hydroxy-17-methyl-,(5a,17b)-.
17b-Hydroxy-17-methyl-2-oxa-5a-androstan-3-one [53-39-4].
»Oxandrolone contains not less than 97.0percent and not more than 100.5percent of C19H30O3,calculated on the dried basis.
Packaging and storage—
Preserve in well-closed,light-resistant containers.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Prepare a solution in chloroform containing 5mg per mL.Apply 10µLeach of this solution and a solution of USP Oxandrolone RSin chloroform,containing 5mg per mLto a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel.Allow the spots to dry,and develop the chromatogram in a solvent system consisting of a mixture of chloroform and methanol (19:1)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.Locate the spots on the plate by lightly spraying with dilute sulfuric acid (1in 2)and heating on a hot plate or under a lamp until spots appear:the RFvalue of the principal spot obtained from the test solution corresponds to that obtained from the Standard solution.
Specific rotation á781Sñ:
between -18
and -24.
and -24.
Test solution:
10mg per mL,in chloroform.
Loss on drying á731ñ—
Dry it at 105for 3hours:it loses not more than 1.0%of its weight.
for 3hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ:
not more than 0.2%.
Ordinary impurities á466ñ—
Test solution:
methanol.
Standard solution:
methanol.
Application volume:
10µL.
Eluant:
a mixture of toluene and isopropyl alcohol (90:10),in a nonequilibrated chamber.
Visualization:
5.
Organic volatile impurities,Method Vá467ñ:
meets the requirements.
Solvent—
Use dimethyl sulfoxide.
Assay—
Transfer about 500mg of Oxandrolone,accurately weighed,to a 250-mLconical flask,and add 25.0mLof 0.1Nalcoholic potassium hydroxide VS.Insert into the neck of the flask,by means of a perforated stopper,an air condenser consisting of a glass tube 70to 80cm in length and 5to 8mm in diameter,and heat the flask on a steam bath for 30minutes,frequently rotating the contents.Cool,add 1mLof phenolphthalein TS,and titrate the excess alkali with 0.1Nhydrochloric acid VS.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nalcoholic potassium hydroxide is equivalent to 30.64mg of C19H30O3.
Auxiliary Information—
Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1426
Pharmacopeial Forum:Volume No.30(1)Page 148
Phone Number:1-301-816-8139