Background:
In the view of the current FDA standardization and product quality control criteria, Quality by
design approach for analytical methods gaining importance to develop a robust analytical method. A new Quality by
Design approach by RP-HPLC was developed and validated for the quantification and purification of Tadalafil
hydrochloride and its tablet formulations.
Objective:
The objective of the study was to develop and validate a simple, robust, and accurate method by QbD approach
for detection Tadalafil hydrochloride and its degradation products in bulk drug and tablet formulation.
Materials and Methods:
The chromatographic separation was performed on JASCO Crest Pack RPC18 column
(250mm×4.6mm, 5μm) with a mobile phase consisting of a mixture of mobile phase A: Acetonitrile: Methanol (40:20 v/
v) and mobile phase B: 0.01M Ammonium acetate in water adjusted pH 3.50± 0.05 with glacial acetic acid with 1.0ml/
min flow rate at 285nm. Box-Behnken's three-level 3 factorial design was employed to create and analyze a "Design
Space" (DoE). This design was statistically analyzed by ANOVA, counter-plot, and 3D response surfaces plots which
demonstrated that the model is statically significant. The developed method was validated as per ICH guidelines Q2 (R1).
Results and Discussion:
The tadalafil hydrochloride showed good regression (R2>0.9995) within test ranges, and the
percent recovery was found to be 98% in marketed formulation.
Conclusion:
The method was found to be highly specific without the interference of impurities and degradation products
of tadalafil hydrochloride. For quantification and routine quality control of tadalafil and its marketed formulation, the
stability-indicating the RP-HPLC method could thus be extended.
Analytical quality by design approach for estimating rosuvastatin calcium in pharmaceutical formulation by green HPLC method: Ecologically evaluated and stability-indicating
