title: Simple 1H NMR spectroscopic method for assay of salts of the contrast agent diatrizoate in commercial solutions.
abstract: A simple, accurate, and specific 1H NMR spectroscopic method was developed for the assay of diatrizoate meglumine or the combination diatrizoate meglumine and diatrizoate sodium in commercial solutions for injection. A mixture of injectable solution and sodium acetate, the internal standard, was diluted with D2O and the 1H NMR spectrum of the solution was obtained. Two approaches were used to calculate the drug content, based on the integral values for the -N-CO-CH3 protons of diatrizoic acid at 2.23 ppm, and -N-CH3 protons of meglumine at 2.73 ppm, and the CH3-CO-protons of sodium acetate at 1.9 ppm. Recoveries (mean +/- standard deviation) of diatrizoic acid and meglumine from 10 synthetic mixtures of various amounts of these compounds with a fixed amount of internal standard were 100.3 +/- 0.55% and 100.1 +/- 0.98%, respectively. In addition to providing a direct means of simultaneously assaying diatrizoic acid and meglumine, the proposed NMR method can also be used to identify diatrizoate meglumine and each of its molecular components.
authors: US Food and Drug Administration, Northeast Regional Laboratory, Brooklyn, NY 11232, USA.
authors: G M
authors: GM
authors: Hanna
authors: C A
authors: CA
authors: Lau-Cam
mesh_terms: D003287:Contrast Media / Q000032:analysis*; D003973:Diatrizoate / Q000032:analysis* / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy; D008536:Meglumine / Q000032:analysis* / Q000737:chemistry; D012015:Reference Standards; D012996:Solutions
chemical_list: D003287:Contrast Media; D012996:Solutions; D003973:Diatrizoate; D008536:Meglumine