A VALIDATED GRADIENT STABILITY-INDICATING LC METHOD FOR THE ANALYSIS OF VALSARTAN IN PHARMACEUTICAL DOSAGE FORM
Objective: The objective of this research work was to develop a sensitive, precise, specific, linear and stability-indicating gradient HPLC method for the estimation of valsartan in bulk drug and in pharmaceutical preparations.
Methods: Chromatographic separation was achieved on C-18 stationary phase with a gradient mobile phase consisting of orthophosphoric acid buffer (the pH of the solution was adjusted to 4.2Â±0.05 with triethylamine) and methanol. The eluent was monitored with PDA detector at 225 nm with a flow rate of 1.0 ml/min, run time of 65 min.
Results: The method was linear over the range of 20-120Î¼g/ml. The correlation coefficient was found to be 0.9994Â±0.02. In order to check the selectivity of the method for pharmaceutical preparations, forced degradation studies were carried out. Valsartan was found to be stable at light and oxidation experiments. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision and robustness. .The LOQ was found to be 0.26Âµg/ml and the LOD was found to be 0.79Âµg/ml. Valsartan showed good correlation coefficient in the concentration range of 20-120Î¼g/ml. The developed method was compared statistically by applying two-way anova and student's t-test to correlate with an isocratic method and was applied to bulk drug and tablet dosage form. There was no significant difference between the two methods.
Conclusion: The proposed method was found to be accurate, precise, sensitive and robust. Hence, it can be used successfully for the routine analysis of valsartan in pharmaceutical formulation and for analysis of stability samples obtained during accelerated stability study.
2. Kumari B, Garg R. Drug profile of valsartan: a review. World J Pharm Sci 2015;3:1598-606.
3. KoÃ§yiÄŸit KB, Unsalan S, Rollas S. Determination and validation of ketoprofen, pantoprazole and valsartan together in human plasma by high-performance liquid chromatography. Pharmazie 2006;61:586-9.
4. Daneshtalab N, Lewanczuk RZ, Jamali F. High performance liquid chromatographic analysis of angiotensin II receptor antagonist valsartan using a liquid extraction method. J Chromatogr B: Anal Technol Biomed Life Sci 2002;766:345-9.
5. GonzÃ¡lez L, LÃ³pez JA, Alonso RM, JimÃ©nez RM. Fast screening method for the determination of angiotensin II receptor antagonists in human plasma by high-performance liquid chromatography with fluorimetric detection. J Chromatogr A 2002;949:49-60.
6. Koseki N, Kawashita H, Haraa H, Niina M, Tanaka M, Kawai R, et al. Development and validation of a method for quantitative determination of valsartan in human plasma by liquid chromatography-tandem mass spectrometry. J Pharm Biomed Anal 2007;43:1769-74.
7. Hao L, Yingwu W, Yao J, Yunbiao T, Jiang W, Limei Z, et al. A liquid chromatography/tandem mass spectrometry method for the simultaneous quantification of valsartan and hydrochlorothiazide in human plasma. J Chromatogr B: Anal Technol Biomed Life Sci 2007;852:436-42.
8. Selvan PS, Gowda KV, Mandal U, Solomon WDS, Pal TK. Simultaneous determination of fixed dose combination of nebivolol and valsartan in human plasma by liquid chromatographic-tandem mass spectrometry and its application to pharmacokinetic study. J Chromatogr B: Anal Technol Biomed Life Sci 2007;858:143-50.
9. Jing N, Bingren X, Yuqi F, Danhua W. Isolation and identification of process impurities in crude valsartan by HPLC, mass spectrometry, and nuclear magnetic resonance spectroscopy. J Liq Chromatogr Relat Technol 2006;29:553-68.
10. Macek J, KlÃma J, PtÃ¡cek P. Rapid determination of valsartan in human plasma by protein precipitation and high-performance liquid chromatography. J Chromatogr B: Anal Technol Biomed Life Sci 2006;832:169-72.
11. Hillaert S, Bossche VW. Simultaneous determination of hydrochlorothiazide and several angiotensin-II-receptor antagonists by capillary electrophoresis. J Pharm Biomed Anal 2003;31:329-39.
12. Satana E, Altmay S, GÃ¶ger NG, Ã–zkan SA, SentÃ¼rk Z. Simultaneous determination of valsartan and hydrochlorothiazide in tablets by first-derivative ultraviolet spectrophotometry and LC. J Pharm Biomed Anal 2001;25:1009-13.
13. Tatar S, SaÄŸlÃk S. Comparison of UV-and second derivative-spectrophotometric and LC methods for the determination of valsartan in a pharmaceutical formulation. J Pharm Biomed Anal 2002;30:371-5.
14. Agrahari V, Kabra V, Gupta S, Nema RK, Nagar M, Karthikeya C, et al. Determination of inherent stability of valsartan by stress degradation and its validation by HPLC. Int J Pharm Clin Res 2009;1:77-81.
15. Bhatia M Sudesh, Kokil S Uttamrao. Determination and validation of valsartan and its degradation products by isocratic HPLC. J Chem Metal 2009;3:1-12.
16. Sharma T, Moitra SK, Si SC, Sankar DG. Development and validation of a HPLC method for the determination of valsartan and its degradation products in a pharmaceutical formulation. Int J Pharm Pharm Sci 2012;4:299-303.
17. ICH. Stability Testing of New Drug Substances and Products. International Conference on Harmonization, IFPMA, Geneva; 2003.