Busulfan
;)
1,4-Butanediol,dimethanesulfonate.
1,4-Butanediol dimethanesulfonate [55-98-1].
»Busulfan contains not less than 98.0percent and not more than 100.5percent of C6H14O6S2,calculated on the dried basis.
Packaging and storage—
Preserve in tight containers.
Labeling—
The label bears a warning that great care should be taken to prevent inhaling particles of Busulfan and exposing the skin to it.
Identification—
A:
Fuse about 100mg with about 100mg of potassium nitrate and a pellet of potassium hydroxide weighing approximately 250mg.Cool,dissolve the residue in water,acidify with 3Nhydrochloric acid,and add a few drops of barium chloride TS:a white precipitate is formed.
B:
To 100mg add 10mLof water and 5mLof 1Nsodium hydroxide.Heat until a clear solution is obtained:an odor characteristic of methanesulfonic acid is perceptible.
C:
Cool the solution obtained in Identificationtest B,and divide it into two equal portions.To one portion add 1drop of potassium permanganate TS:the purple color changes to violet,then to blue,and finally to emerald-green.Acidify the second portion of the solution with 2Nsulfuric acid,and add 1drop of potassium permanganate TS:the color of the permanganate is not discharged.
Loss on drying á731ñ—
Dry it in vacuum at 60
to 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.
Residue on ignition á281ñ:
not more than 0.1%.
Organic volatile impurities,Method Vá467ñ:
meets the requirements.
Solvent—
Use dimethyl sulfoxide.
Assay—
Transfer about 80mg of Busulfan,accurately weighed,to a 250-mLconical flask.Add about 30mLof water,swirl,add phenolphthalein TS,and neutralize with 0.05Nsodium hydroxide.Connect the flask to a reflux air condenser,and boil the mixture gently for not less than 30minutes,adding water occasionally to maintain the volume.Cool to room temperature,add phenolphthalein TS,and titrate with 0.05Nsodium hydroxide VS.Each mLof 0.05Nsodium hydroxide is equivalent to 6.158mg of C6H14O6S2.
Auxiliary Information—
Staff Liaison:Lawrence Evans,III,Ph.D.,Scientist
Expert Committee:(PA6)Pharmaceutical Analysis 6
USP28–NF23Page 300
Phone Number:1-301-816-8389