ONE STEP QUANTIFICATION ANALYTICAL METHOD AND CHARACTERIZATION OF VALSARTAN BY LC-MS

Abstract

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 ×4.0 mm, 5 µm. 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).