A Validated Stability-Indicating High-Performance Thin-Layer Chromatographic Method for the Estimation of Pirfenidone in Tablet Formulation

Abstract Background A sensitive, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been developed for the analysis of Remogliflozin etabonate in tablet formulation. HPTLC plates precoated with silica gel 60 F254 were used as the stationary phase; methanol: ethyl acetate: toluene: NH3 (2:4:4:0.1, v/v/v) was used as mobile phase, and densitometry was used for the quantitative estimation of the drug. The proposed method was validated with respect to linearity, accuracy, precision, and robustness and applied for the estimation of drug in tablet dosage form. Results The Rf value of Remogliflozin etabonate was observed to be 0.61. The densitometric estimation was performed in reflectance mode at 229 nm. The method was found to be linear in the range of 500–8000 ng/band for Remogliflozin etabonate. The possible degradation pathway was estimated by performing forced degradation studies. The degradant peaks were well resolved from the drug peak with acceptable resolution in their Rf value. Conclusion An accurate and precise high-performance thin-layer chromatographic method has been developed for the quantification of Remogliflozin etabonate in tablets. Forced degradation studies were performed, and drug was found to be highly susceptible to acid, base hydrolysis, and oxidative stress degradation and gets converted into active drug Remogliflozin. Both Remogliflozin etabonate and Remogliflozin bands were well resolved. The method was applied for the analysis of drug in tablet formulation, and it can be used for routine quality control analysis, as well as for the analysis of stability samples.

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VALIDATED STABILITY INDICATING HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR REPAGLINIDE API

INDIAN DRUGS ◽

10.53879/id.52.09.10162 ◽

2015 ◽

Vol 52 (09) ◽

pp. 48-54

Author(s):

P. P. Thakkar ◽

◽

N. R Patel ◽

C. S Kothari ◽

R Patel ◽

...

Keyword(s):

Thin Layer ◽

High Performance ◽

Chromatographic Method ◽

Degradation Products ◽

Linear Regression Analysis ◽

Tablet Formulation ◽

Content Uniformity ◽

Calibration Data ◽

Stability Indicating ◽

Photolytic Degradation

A simple, precise and accurate stability-indicating high performance thin layer chromatographic method for estimation of repaglinide in bulk drug and in tablet formulation has been developed and validated. The stationary phase used was HPTLC plates precoated with silica gel 60F254 using the mobile phase of chloroform: methanol: ammonia (4.5:1.0:0.05 V/V/V). Densitometric analysis was performed in absorbance mode at 242 nm. The method showed compact bands of drug at RF value of 0.31 ± 0.02. Linear Regression analysis of calibration data showed good linear relationship with r2= 0.9981 in concentration range of 500 - 3000 ng/band. Drug was subjected to ICH-prescribed stress conditions such as acid, base, peroxide, thermal and photolytic degradation and method was found able to separate the peaks for all degradation products from analyte peak. Validation of the developed method was carried out for its specificity, linearity, range, precision, accuracy and robustness. The method was further applied for repaglinide estimation in pharmaceutical tablet formulation and it was found to be reliable. The method was also used successfully to carry out content uniformity test of repaglinide in tablet dosage form.

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