Powdered Digitalis
»Powdered Digitalis is Digitalis dried at a temperature not exceeding 60,reduced to a fine or a very fine powder,and adjusted,if necessary,to conform to the official potency by admixture with sufficient Lactose,Starch,or exhausted marc of digitalis,or with Powdered Digitalis having either a lower or a higher potency.
The potency of Powdered Digitalis is such that,when assayed as directed,100mg is equivalent to 1USP Digitalis Unit.*
NOTE—When Digitalis is prescribed,Powdered Digitalis is to be dispensed.
Packaging and storage— Preserve in tight,light-resistant containers.Apackage of a suitable desiccant may be enclosed in the container.
Identification—
A: It conforms to the description for Ground Digitalisin the section Botanic characteristicsunder Digitalis.
B: Transfer 100mg to a 15-mLcentrifuge tube containing 2.0mLof diluted alcohol and 1.0mLof lead acetate TS,mix,shake,and boil for 2minutes.Centrifuge,decant the supernatant into a second 15-mLcentrifuge tube,add 2.0mLof chloroform,and mix.Centrifuge,then remove the lower layer,and filter it through a chloroform-washed small column of anhydrous sodium sulfate (100to 300mg)into a 5-mLcentrifuge tube.Evaporate the chloroform solution under a stream of nitrogen to dryness,and dissolve the residue in 100µLof a mixture of methanol and chloroform (1:1).Prepare a Standard solution in the same manner,using 100mg of USP Digitalis RS(Standard solution A).Prepare a second Standard solution by dissolving USP Digitoxin RSand USP Gitoxin RSin a mixture of methanol and chloroform (1:1)such that the final concentration of each is approximately 0.2mg per mL(Standard solution B).Apply 10µLof the test solution,10µLof Standard solution A,and 10µLof Standard solution B,each as a narrow band about 15mm long,to a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture,and allow the bands to dry.Develop the chromatogram in a saturated chamber,using a solvent system consisting of a mixture of ethyl acetate,methanol,and water (30:4:3)until the solvent front has moved about 15cm from the origin.Mix 10mLof chloramine Tsolution (3in 100)with 40mLof a 1in 4solution of trichloroacetic acid in alcohol (store the mixture in a cool place,and use it within 1week),and spray the air-dried chromatographic plate with this mixture.Heat the plate at 110for 15to 20minutes,and examine it under long-wavelength UVlight.Locate the 2prominent bands obtained from Standard solution Acorresponding in RFvalue to the 2bands obtained from Standard solution B.The chromatogram obtained from the solution under test shows bands corresponding to them,and also shows bands corresponding to the 3other bands most prominent in the chromatogram from Standard solution Abut of lower RFvalue.Relative RFvalues for the 5bands are:1.0(digitoxin);0.8to 0.9(gitoxin);0.6to 0.7;0.4to 0.5;and 0.3to 0.4.
Microbial limits á61ñ It meets the requirements of the test for absence of Salmonellaspecies.
Acid-insoluble ash á561ñ: not more than 5.0%.
Organic volatile impurities,Method IVá467ñ: meets the requirements.
Assay— Proceed with Powdered Digitalis as directed in the Assayunder Digitalis.
The potency of Powdered Digitalis,calculated from that of the Assay preparation,is satisfactory if the result is not less than 0.85USP Digitalis Unit and not more than 1.20USP Digitalis Units per 100mg.

*  One USP Digitalis Unit represents the potency of 100mg of USP Digitalis RS.
Auxiliary Information— Staff Liaison:Gabriel I.Giancaspro,Ph.D.,Senior Scientist and Latin American Specialist
Expert Committee:(DSB)Dietary Supplements:Botanicals
USP28–NF23Page 641
Phone Number:1-301-816-8343