RP-HPLC method development and validation of capecitabine in bulk drug and formulation
DOI:
https://doi.org/10.61096/ijpar.v5.iss1.2016.190-198Keywords:
Capecitabine, RP-HPLC Method Development, Validation.Abstract
Objective
To Develop and validate a simple, selective, rapid, precise and accurate High Performance Liquid Chromatographic Method for determination of capecitabine in bulk and its pharmaceutical formulation product.
Method
RP-HPLC method was performed by using a mobile phase consisting mixture of Methanol and Ammonium acetate buffer (pH 4.5) in the proportion 60:40v/v. A ZORBAX Eclipse plus C18 (4.6 ×100mm, 3.5μ) column was used as a stationary phase. . HPLC analysis of Capecitabine was carried out at a wavelength of 241nm with a flow rate of 1ml/min.
Results
The linear regression analysis data for the calibration curve showed a good linear relationship with a correlation coefficient 0.9984. The linear regression equation was
y=3726540. 2 x+27390388. 1. This was found to give a sharp peak of Capecitabine at a retention time of 2.77min.Validation parameters were evaluated for the method according to the ICH (Q2R1) guidelines. The limit of detection and limit of quantification for the method were 0.6721μg/mL and 1.9989μg/mL, respectively. The %RSD values for Intra-day precision and Inter-day precision were found to be 0.31 % and 0.30% respectively. Accuracy of the method was determined through recovery studies which were found to be within 97.57-102.22%.
Conclusion
The method was validated for system suitability, accuracy, precision, robustness and ruggedness. The precision, accuracy, sensitivity, short retention time and composition of the mobile phase indicated that this method is better than the earlier methods developed for the quantification of Capecitabine.
