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 95.0 percent and not more than 105.0 percent 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.
USP Reference standards 11
A: Dilute a volume of Solution, if necessary, with an 0.8 in 1000 solution of sodium hydroxide in methanol, to obtain a test solution having a concentration of 1 mg per mL. The test solution responds to the Thin-Layer Chromatographic Identification Test 201, the Standard solution being prepared at a concentration of 1 mg of USP Diatrizoic Acid RS per mL in a 0.8 in 1000 solution of sodium hydroxide in methanol, the solvent mixture being a mixture of chloroform, methanol, and ammonium hydroxide (20:10:2), and short-wavelength UV light being used to locate the spots.
B: Evaporate a volume of Solution, equivalent to about 500 mg of diatrizoate meglumine and diatrizoate sodium, to dryness, and heat the residue so obtained in a crucible: violet vapors are evolved.
pH 791: between 6.0 and 7.6.
Iodine and iodide Using as the Test preparation a volume of Solution equivalent to about 2 g of diatrizoate meglumine and diatrizoate sodium and diluting it with water to 24 mL in a 50-mL centrifuge tube provided with a stopper, proceed as directed for Procedure in the test for Iodine and iodide under Diatrizoate Meglumine.
Assay for diatrizoate meglumine Pipet a volume of Solution, equivalent to about 1.5 g of diatrizoate meglumine and diatrizoate sodium, into a 250-mL volumetric flask, dilute with water to volume, and mix. Pipet 10 mL of the solution so obtained into a glass-stoppered, 250-mL flask. Add 4 mL of 2 N sulfuric acid and 20 mL of sodium metaperiodate solution (1 in 200). Insert the stopper, and set aside in the dark for 1 hour. Add 50 mL of water, mix, and add 10 mL of potassium iodide TS. Insert the stopper quickly, mix by swirling for 20 seconds, and immediately titrate with 0.1 N sodium thiosulfate VS, using 3 mL of starch TS. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N sodium thiosulfate is equivalent to 10.11 mg of C11H9I3N2O4·C7H17NO5.
Assay for iodine Transfer an accurately measured volume of Solution, equivalent to about 4 g of the total of diatrizoate meglumine and diatrizoate sodium, to a 50-mL volumetric flask, dilute with water to volume, and mix. Pipet 5 mL of this solution into a glass-stoppered, 125-mL conical flask, add 30 mL of 1.25 N sodium hydroxide and 500 mg of powdered zinc, connect the flask to a reflux condenser, and reflux the mixture for 1 hour. Cool the flask to room temperature, rinse the condenser with 20 mL of water, disconnect the flask from the condenser, and filter the mixture. Rinse the flask and filter thoroughly, adding the rinsings to the filtrate. Add 5 mL of glacial acetic acid and 1 mL of tetrabromophenolphthalein ethyl ester TS, and titrate with 0.05 N silver nitrate VS until the yellow precipitate just turns green. Each mL of 0.05 N silver nitrate is equivalent to 6.345 mg of iodine.
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USP35NF30 Page 2866Pharmacopeial Forum: Volume No. 27(6) Page 3273