DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING HPTLC METHOD FOR VERAPAMIL ANALYSIS USING THE AQBD APPROACH
DOI:
https://doi.org/10.22159/ijap.2025v17i6.54435Keywords:
HPTLC, Verapamil, Stability-indicating method, Analytical quality by design (AQbD), Method validationAbstract
Objective: To develop selective, precise and accurate High Performance Thin Layer Chromatography (HPTLC) method for forced degradation study of Verapamil by implementing AQbD (Analytical quality by design) approach. To optimize chromatographic conditions and detection wavelength for efficient separation and quantification of Verapamil using AQbD. To perform a forced degradation study on Verapamil as per International Council for Harmonisation (ICH) guideline. To validate the developed HPTLC method as per ICH Q2(R2) guideline.
Methods: The method employs TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The mobile phase consists of toluene, ethyl acetate, methanol, and ammonia in a volumetric ratio of 4:2:3.5:0.5. Verapamil quantification was performed in reflective mode at a wavelength of 276 nm. The method was validated for linearity, precision, accuracy, recovery, and robustness.
Results: The HPTLC method exhibited strong retention for verapamil with an Rf value of 0.72. Calibration curve analysis demonstrated excellent linearity over a concentration range of 200-1000 ng/band with a correlation coefficient (R²) of 0.9961. The slope and intercept were determined as 0.0013x+0.0074. The detection and quantitation limits were found to be 0.3008 ng/band and 0.9116 ng/band, respectively. The method showed high precision, accuracy, and robustness, ensuring its reliability for pharmaceutical applications.
Conclusion: The validated HPTLC method provides an efficient and reliable approach for the quantitative analysis of verapamil in synthetic mixtures. Its precision, sensitivity, and rapid analytical capabilities make it a suitable technique for pharmaceutical quality control and routine analysis.
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