Stability-indicating Liquid Chromatographic Assay Method Research Articles

A sensitive and specific high-performance thin-layer chromatography-densitometry method for determination of Rebamipide in the bulk material and in pharmaceutical formulation

Rebamipide (RBP), α((4-chlorobenzoyl)-amino)-1,2-dihydro-2-oxo-4-quinoline propanoic acid is antiulcer (gastric cytoprotectant). Literature survey revealed many reverse-phase high-performance liquid chromatography (RP-HPLC) methods for determination of RBP in human plasma, rat plasma, and coionic tissue. Stability-indicating liquid chromatographic assay method and first-order derivative spectrophotometric methods have been established for the determination of RBP in bulk and tablet dosage form. Nowadays, high-performance thin-layer chromatography (HPTLC) is becoming a routine analytical technique due to its low operating cost, high sample throughput, and need for minimum sample clean up. The major advantage of HPTLC is that several samples can be run simultaneously using a small quantity of mobile phase unlike HPLC, thus lowering analysis time and cost per analysis. The intention of the present work is to establish simple, precise, and accurate stability-indicating densitometric thin-layer chromatography (TLC)-densitometry method for analysis of RBP in the bulk material and in tablets. Further the developed method has to be validated as per the International Conference on Harmonisation (ICH) guidelines.

Optimization of Forced Degradation Using Experimental Design and Development of a Stability-Indicating Liquid Chromatographic Assay Method for Rebamipide in Bulk and Tablet Dosage Form

A novel stability-indicating RP-HPLC assay method was developed and validated for quantitative determination of rebamipide in bulk and tablet dosage form. Rebamipide (drug and drug product) solutions were exposed to acid and alkali hydrolysis, thermal stress, oxidation by hydrogen peroxide and photodegradation. Experimental design has been used during forced degradation to determine significant factors responsible for degradation and to obtain optimal degradation conditions. In addition, acid and alkali hydrolysis was performed using a microwave oven. The chromatographic method employed the HiQ sil C-18HS (250 × 4.6 mm; 5 μm) column with mobile phase consisting of 0.02 M potassium phosphate (pH adjusted to 6.8) and methanol (40:60, v/v) and the detection was performed at 230 nm. The procedure was validated for specificity, linearity, accuracy, precision and robustness. There was no interference observed of excipients and degradation products in the determination of the active pharmaceutical ingredient. The method showed good accuracy and precision (intra and inter day) and the response was linear in a range from 0.5 to 5 μg mL−1. The method was found to be simple and fast with less trial and error experimentation by making use of experimental design. Also, it proved that microwave energy can be used to expedite hydrolysis of rebamipide.