C15H14NNaO3·2H2O 315.30

1H-Pyrrole-2-acetic acid, 1-methyl-5-(4-methylbenzoyl)-, sodium salt, dihydrate.
Sodium 1-methyl-5-p-toluoylpyrrole-2-acetate dihydrate [64490-92-2].

Anhydrous 279.27 [35711-34-3].

Packaging and storage— Preserve in well-closed containers.

USP Reference standards 11— USP Tolmetin Sodium RS.

Identification—

Loss on drying 731— Dry it in vacuum at 60 for 4 hours: it loses between 10.4% and 12.4% of its weight.

Heavy metals, Method II 231: 0.002%.

Chromatographic purity— Dissolve 125 mg in 10 mL of methanol to obtain the Test solution. Dissolve USP Tolmetin Sodium RS in methanol to obtain a Standard solution having a concentration of 12.5 mg per mL. Dilute a portion of this Standard solution quantitatively with methanol to obtain a Diluted standard solution having a concentration of 62.5 µg per mL. Apply separate 20-µL portions of the three solutions on the starting line to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with 0.25-mm layer of chromatographic silica gel mixture. Develop the chromatogram in a solvent system consisting of a mixture of chloroform and glacial acetic acid (95:5) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the chamber, mark the solvent front, air-dry, and view under short-wavelength UV light: the RF value of the principal spot from the Test solution corresponds to that from the Standard solution. Any other spot obtained from the Test solution does not exceed in size or intensity the principal spot obtained from the Diluted standard solution (0.5%), and the sum of the total impurities based on a comparison of the intensities of all such other spots with the Diluted standard solution does not exceed 2.0%.

Organic volatile impurities, Method I 467: meets the requirements.

Residual solvents 467: meets the requirements.

Assay— Dissolve, by warming, about 300 mg of Tolmetin Sodium, accurately weighed, in 150 mL of glacial acetic acid. Cool to room temperature, and titrate with 0.1 N perchloric acid VS, determining the endpoint electrometrically. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 27.93 mg of C15H14NNaO3.

Expert Committee : (MDCCA05) Monograph Development-Cough Cold and Analgesics

USP29–NF24 Page 2173

Phone Number : 1-301-816-8139