Development and validation of a stability indicating high performance liquid chromatography method for trimethobenzamide

Abstract

A simple, accurate, precise and robust stability indicating RP-HPLC assay method has been developed for the estimation of trimethobenzamide in stress sample. An isocratic separation of trimethobenzamide was achieved on Kromasil 100 C-18 column (250 X 4.6mm, 5μ) with a flow rate of 1.0 ml/min and by using a photodiode array detector to detect the analyte at 213nm. The optimized mobile phase consisted of methanol: ammonium formate (44:56, v/v). The drug was subjected to different forced degradation conditions according to ICH guidelines including acid, base, neutral hydrolysis, oxidation, photolysis and thermal degradation. Degradation products were found only in basic and oxidative degradation conditions. All the degradation products got eluted in an overall analytical run time of 12min. The developed analytical method has been validated according to the ICH guidelines. Response of trimethobenzamide was linear over the concentration range of 0.5-50μg/ mL (r 2 = 0.999). Accuracy was found to be in between 94.03% to 100.39%. Degradation products resulting from the stress studies did not interfere with the detection of the analyte.

Establishment of a Rapid and Highly Sensitive Reverse-phase High-performance Liquid Chromatography Based Analytical Assay Method for Duvelisib

“…23 ICH Q2 R1 and AOAC guidelines were followed for setting the acceptance criteria of the validation study. 24…”

Identification and structural characterization of potential degradation products of baricitinib using liquid chromatography combined with quadrupole time-of-flight mass spectrometry

“…Degradation of BRT was achieved under all tested stress conditions, however, no data regarding the DPs are given. Furthermore, a comprehensive study describes the isolation and identification of three new process related impurities of BRT using HPLC technique, while their structures were further confirmed using 1 H NMR, 13 C NMR and mass spectrometry techniques [6].…”

“…Advanced analytical techniques like reverse phase high performance liquid chromatography (RP-HPLC) coupled with tandem mass spectrometry (MS/MS) and nuclear magnetic resonance (NMR) spectroscopy are applied vastly for the detection and structure elucidation of all kinds of organic impurities [8,[10][11][12][13][14][15][16].…”