DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF AZILSARTAN MEDOXOMIL AND CHLORTHALIDONE IN BULK AND TABLET DOSAGE FORM
Objective: A simple, precise, accurate method was developed for the simultaneous estimation of azilsartan and chlorthalidone in bulk and tablet dosage form by RP-HPLC technique.
Methods: Acetonitrile and water in the ratio of (70:30) pH 2.8 used as mobile phase run through (Cosmosil C18 (4.6ID x 250 mm, Particle size: 5 micron) column with a flow rate of 0.9 ml/min. The temperature of the column oven was maintained at 30 Â°C. Wavelength was selected 244 nm. Stock and working solutions were prepared by using the diluents water and acetonitrile in the ratio of 50:50. Runtime was fixed to 9 min.
Results: Chlorthalidone and azilsartan were eluted at 2.02 and 3.92 with good resolution the plate count, tailing factor and all system suitability parameters are within ICH range. Azilsartan Medoxomil and Chlorthalidone were found to be linear low in concentration range of 80-400Î¼g/ ml and 25-125Î¼g/ ml respectively in the linearity study, regression equation and coefficient of correlation for Azilsartan Medoxomil and Chlorthalidone were found to be (y = 28695x+15397 rÂ²=0.995) and (y=13444+27405 rÂ² = 0.996) Percentage recovery for both Azilsartan Medoxomil and Chlorthalidone was found in range of 99.89%-99.96% indicating accuracy of the proposed work. Assay of the tablet was performed and found as 100.15%.Conclusion: All the parameters were within the ICH guidelines, and the method was economical and simple as retention times were less than in literature and decreased run time.
2. Bakris Gl, Sica D, Weber M, White WB, Roberts A, Prez A, et al. The comparative effects of azilsartan medoxomil and chlorthalidone on ambulatory and clinical blood pressure. J Clin Hypertension (Green Wich) 2011;13:81-8.
3. USP 25-NF 20, â€œValidation of conmpendial Methods Section (1225) (United States Pharmacopoeial Conventionâ€, Rockville, Maryland, USA; 2002. p. 2256.
4. Madhu Babu, Kasimala Bikshal Babu Kasimala. RP-HPLC method development and validation for the simultaneous estimation of Azilsartan medoxomil and Chlortalidone in pharmaceutical dosage forms. Am J PharmTech Res 2012;2:117-26.
5. GA Shabir. Validation of high-performance liquid chromatography methods for pharmaceutical analysis Understanding the differences and similarities between the validation requirements of the US Food and Drug Administration, the US Pharmacopeia and the International Conference on Harmonization. J Chromatography A 2003;987:57â€“66w.
6. Requirements of FDA, the US pharmacopeia and the ICH. J Chromatography A 2003;987:57-66.
7. International Conference on Harmonization, "Q2A: Text on Validation of Analytical Procedures. Federal Register 1995;60:11260â€“2.
8. International Conference on Harmonization, "Q2B: Validation of analytical procedures: Methodology. Federal Register 1996; 62:27463â€“7.
9. FDA approves Edarbi to treat high blood pressure. (Press release). U. S. Food and Drug Administration (FDA); 2011.
10. http://www.drugs.com/azilsartan-medoxomil.html. [Last accessed