Saccharin Sodium Tablets
»Saccharin Sodium Tablets contain the equivalent of not less than 95.0percent and not more than 110.0percent of the labeled amount of saccharin (C7H5NO3S).
Packaging and storage— Preserve in well-closed containers.
Completeness of solution— Place 5Tablets in a 250-mLbeaker containing 150mLof water at 25.Stir for 5minutes:all of the Tablets dissolve to give a clear or practically clear solution.
Change to read:
Identification—
A:USP28 Dissolve a quantity of Tablets,equivalent to about 1g of saccharin,in 10mLof water,filter if necessary,and to the solution add 5mLof 3Nhydrochloric acid:a white precipitate of saccharin is formed.Collect the precipitate on a filter,wash with small portions of cold water until the last washing is practically free from chloride,and dry it at 105for 2hours:the saccharin so obtained melts between 226and 230,the procedure for Class Ibeing used (see Melting Range or Temperature á741ñ).
[NOTE—Use also in Identificationtests Band C.]
B: Dissolve about 100mg in 5mLof sodium hydroxide solution (1in 20),evaporate to dryness,and gently fuse the residue over a small flame until it no longer evolves ammonia.Allow the residue to cool,dissolve in 20mLof water,neutralize with 3Nhydrochloric acid,and filter:the addition of a drop of ferric chloride TSto the filtrate produces a violet color.
C: Mix 20mg with 40mg of resorcinol,add 10drops of sulfuric acid,and heat the mixture in a suitable liquid bath of 200for 3minutes.Allow it to cool,and add 10mLof water and an excess of 1Nsodium hydroxide:a fluorescent green liquid results.USP28
Limit of ammonium salts— Dissolve a quantity of powdered Tablets,equivalent to about 300mg of saccharin,in 5mLof water,and warm with 3mLof 1Nsodium hydroxide:the odor of ammonia is not perceptible.
Assay— Weigh and finely powder not fewer than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 100mg of saccharin,to a 100-mLvolumetric flask,add about 50mLof water,agitate until the tablet material is dissolved or evenly dispersed,dilute with water to volume,and mix.Transfer 10.0mLto a separator,add 2mLof 3Nhydrochloric acid,and extract with five 20-mLportions of a solvent composed of chloroform and alcohol (9:1).Collect the combined extracts in a beaker,and evaporate on a steam bath to dryness with the aid of a current of air.Dissolve the residue in 10mLof sodium hydroxide solution (1in 250),transfer the solution with the aid of water to a 200-mLvolumetric flask,dilute with water to volume,and mix.Concomitantly determine the absorbances of this solution and a Standard solution of USP Saccharin RSin the same medium having a known concentration of about 50µg per mL,in 1-cm cells at the wavelength of maximum absorbance at about 269nm,with a suitable spectrophotometer,using water as the blank.Calculate the quantity,in mg,of saccharin (C7H5NO3S)in the portion of Tablets taken by the formula:
(2C)(AU/AS),
in which Cis the concentration,in µg per mL,of USP Saccharin RSin the Standard solution;and AUand ASare the absorbances of the solution from the Tablets and the Standard solution,respectively.
Auxiliary Information— Staff Liaison:Justin Lane,B.S.,Scientific Associate
Expert Committee:(EMC)Excipients:Monograph Content
USP28–NF23Page 1746
Pharmacopeial Forum:Volume No.30(2)Page 536
Phone Number:1-301-816-8323
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