ONE STEP QUANTIFICATION ANALYTICAL METHOD AND CHARACTERIZATION OF VALSARTAN BY LC-MS
Objective: To develop precise LC-MS method for the estimation of valsartan impurities and perform validation as per ICH guidelines.
Methods: Valsartan (VLN) and its degradation products were analyzed by reverse phase high-performance liquid chromatography (RP-HPLC) using mobile phase water: acetonitrile: glacial acetic acid: phosphate buffer in the ratio of 500:500:1:0.5 v/v/v/v at 225 nm using column nucleosil C18, 125 Ã—4.0 mm, 5 Âµm. VLN sample (VLN SPL) thus obtained an unknown major impurity (UIMP) of 0.5 % at 0.38 retention time ratio (RRt) and purity of VLN was found to be 98.70 % respectively.
Results: Estimation of VLN SPL total unknown impurities was found to be 1.3% by RP-HPLC. In similarly by liquid chromatography mass spectroscopy (LC-MS) a typical chromatogram of valsartan (VLN) at Rt 9.03 min and UIMP at Rt 3.3 min were recorded at a total run time of 23 min. Assay of VLN SPL was validated as per international council for harmonization (ICH) guidelines. Average % recovery was found to be 100.04 % for VLN SPL.
Conclusion: The proposed work clearly indicates that the method can be easily adapted for the routine one step estimation of VLN active pharmaceutical ingredient (API).
2. Ulrich B. A high-throughput process for the synthesis of valsartan. Int J Res Pharm Chem 2007;11:892â€“8.
3. N Rama Rao. Pharmaceutical impurities: an overview. Ind J Pharm Edu Res 2010;3:301-10.
4. S Lakshmana Prabu . Impurities and its importance in pharmacy. Int J Pharm Sci Rev Res 2010;2:66-71.
5. Kena H Patel. Simultaneous estimation of sacubitril and valsartan in the synthetic mixture by an RP-HPLC method. J Pharm Sci Bio Sci Res 2016;6:262-9.
6. LRD Bhavani. Method development and validation of HPLC for determination of levetiracetan and valsartan in their formulations. Res Rev J Pharm Anal 2015;2:42-56.
7. Ch Krishnaiah. Stability-indicating UPLC method for determination of valsartan and their degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms. J Pharm Biomed Anal 2010;3:483-9.
8. S Senthil Kumar. A validated gradient stability-indicating LC method for the analysis of valsartan in pharmaceutical dosage form. Int J Pharm Sci 2016;5:128-33.
9. Mittal A. Design of experiment based optimized RP-HPLC method for simultaneous estimation of amlodipine and valsartan in bulk and tablet formulations. Austin J Anal Pharm Chem 2015;6:1-6.
10. Subhajit G. RP-HPLC method for estimation of valsartan in solid oral dosage forms. J Pharm Sci Tech 2014;6:88-91.
11. Sridevi Ramachandran. Stability-indicating HPLC method for simultaneous determination of valsartan and ezetimibe in pharmaceuticals. Trop J Pharm Res 2014;5:809-17.
12. Tripti Sharma. Development and validation of a stability indicating RP-HPLC method for the determination of valsartan. Int J Pharm Sci 2015;7:57-61.
13. Sunil Pai. A simple reverse phase-high-performance liquid chromatography method development and validation of valsartan in bulk and itâ€™s tablet dosage form. Asian J Pharm Clin Res 2017;6:333-7.