A rapid qNMR protocol for the analysis of triclofos sodium in solution state pharmaceutical dosage formulations

Abstract

95-101A quaitative 31P{1H} nuclear magnetic resonance (NMR) spectroscopy has been used for quantification of triclofos sodium (TCFS) in syrup formulations. Its hydrolysis product 2,2,2-trichloroethanol (TCE) has been quantified by 1H NMR spectroscopy. Standard addition to syrup formulations is used for the quantification of these components. Dimethylsulfone (DMS) and hexamethyl benzene-1,3,5-triyltris(methylene)triphosphonate (HMBTP) have been used as internal standards for quantitative 1H NMR and 31P{1H} NMR respectively. All NMR experiments are performed on 400 MHz NMR spectrometer equipped with a room temperature broadband observe probe. The method is simple, rapid, and easy to implement. It also shows excellent accuracy (recoveries for TCFS 98.9-101.5% and TCE 98.6 to 99.9%), linearity (r2>0.99), range, precision, accuracy and robustness. Four commercially available formulations have been subjected to the developed method. The average concentration for TCFS is found to be 93±4 mg/mL in the commercially available drug samples. </span