A stability-indicating proton nuclear magnetic resonance spectroscopic method for the analysis of propantheline bromide in pharmaceutical samples.
A rapid, specific and accurate proton nuclear magnetic resonance (1H NMR) spectroscopic method was developed for the simultaneous quantitative analysis of propantheline bromide and its degradation product, xanthanoic acid, in bulk materials and tablets. 1,3,5-Trinitrobenzene served as an internal standard and deuterochloroform was used as the solvent for the analytical samples. The quantities of propantheline bromide and xanthanoic acid were calculated on the basis of the integrals for signals of the methine proton of propantheline at 5.09 ppm, the methine proton of xanthanoic acid at 4.99 ppm, and the aromatic protons of the internal standard at 9.39 ppm. The accuracy of the method was established through the analysis of synthetic mixtures containing the parent compound, its degradation product and the internal standard. An excellent agreement was verified between the assay results and the quantities of the various compounds in the mixtures. The mean +/- SD recovery values for propantheline bromide and xanthanoic acid from a set of 10 synthetic mixtures were 99.6 +/- 0.8% and 98.9 +/- 1.8%, respectively. The assay of 10 lots of commercial propantheline bromide tablets by 1H NMR spectroscopy indicated drug and degradate contents in the ranges 97.1-99.8% and 0.1-0.9%, respectively. In addition, the proposed analytical method was found suitable for detecting the formation of xanthanoic acid from propantheline bromide in aqueous media in concentrations below 0.1% of that of the parent compound.
Hanna
G M
GM
New York Regional Laboratory, U.S. Food and Drug Administration, Jamaica, New York, USA.
Lau-Cam
C A
CA
D004355:Drug Stability; D007202:Indicators and Reagents; D009682:Magnetic Resonance Spectroscopy; D011413:Propantheline / Q000032:analysis*; D012015:Reference Standards; D012997:Solvents; D013607:Tablets
D007202:Indicators and Reagents; D012997:Solvents; D013607:Tablets; D011413:Propantheline