Diatrizoate Meglumine and Diatrizoate Sodium Solution
»Diatrizoate Meglumine and Diatrizoate Sodium Solution is a solution of Diatrizoic Acid in Purified Water prepared with the aid of Meglumine and Sodium Hydroxide.It contains not less than 95.0percent and not more than 105.0percent of the labeled amounts of diatrizoate meglumine (C11H9I3N2O4·C7H17NO5)and of iodine (I).It may contain small amounts of suitable buffers,Edetate Disodium,and flavoring agents.
Packaging and storage— Preserve in tight,light-resistant containers.
Labeling— Label the container to indicate that the contents are not intended for parenteral use.
Identification—
A: Dilute a volume of Solution,if necessary,with an 0.8in 1000solution of sodium hydroxide in methanol,to obtain a test solution having a concentration of 1mg per mL.The test solution responds to theThin-Layer Chromatographic Identification Test á201ñ,the Standard solution being prepared at a concentration of 1mg of USP Diatrizoic Acid RSper mLin a 0.8in 1000solution of sodium hydroxide in methanol,the solvent mixture being a mixture of chloroform,methanol,and ammonium hydroxide (20:10:2),and short-wavelength UVlight being used to locate the spots.
B: Evaporate a volume of Solution,equivalent to about 500mg of diatrizoate meglumine and diatrizoate sodium,to dryness,and heat the residue so obtained in a crucible:violet vapors are evolved.
pHá791ñ: between 6.0and 7.6.
Iodine and iodide— Using as theTest preparation a volume of Solution equivalent to about 2g of diatrizoate meglumine and diatrizoate sodium and diluting it with water to 24mLin a 50-mLcentrifuge tube provided with a stopper,proceed as directed forProcedure in the test forIodine and iodide underDiatrizoate Meglumine.
Assay for diatrizoate meglumine— Pipet a volume of Solution,equivalent to about 1.5g of diatrizoate meglumine and diatrizoate sodium,into a 250-mLvolumetric flask,dilute with water to volume,and mix.Pipet 10mLof the solution so obtained into a glass-stoppered,250-mLflask.Add 4mLof 2Nsulfuric acid and 20mLof sodium metaperiodate solution (1in 200).Insert the stopper,and set aside in the dark for 1hour.Add 50mLof water,mix,and add 10mLof potassium iodide TS.Insert the stopper quickly,mix by swirling for 20seconds,and immediately titrate with 0.1Nsodium thiosulfate VS,using 3mLof starch TS.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nsodium thiosulfate is equivalent to 10.11mg of C11H9I3N2O4·C7H17NO5.
Assay for iodine— Transfer an accurately measured volume of Solution,equivalent to about 4g of the total of diatrizoate meglumine and diatrizoate sodium,to a 50-mLvolumetric flask,dilute with water to volume,and mix.Pipet 5mLof this solution into a glass-stoppered,125-mLconical flask,add 30mLof 1.25Nsodium hydroxide and 500mg of powdered zinc,connect the flask to a reflux condenser,and reflux the mixture for 1hour.Cool the flask to room temperature,rinse the condenser with 20mLof water,disconnect the flask from the condenser,and filter the mixture.Rinse the flask and filter thoroughly,adding the rinsings to the filtrate.Add 5mLof glacial acetic acid and 1mLof tetrabromophenolphthalein ethyl ester TS,and titrate with 0.05Nsilver nitrate VSuntil the yellow precipitate just turns green.Each mLof 0.05Nsilver nitrate is equivalent to 6.345mg of iodine.
Auxiliary Information— Staff Liaison:Andrzej Wilk,Ph.D.,Senior Scientific Associate
Expert Committee:(RMI)Radiopharmaceuticals and Medical Imaging Agents
USP28–NF23Page 615
Pharmacopeial Forum:Volume No.27(6)Page 3273
Phone Number:1-301-816-8305