A Rapid Novel HPLC Method for Estimation of Eight Related Compounds in Azilsartan Kamedoxomil and Identification of Degradation Compounds by Using LC–MS

Abstract

A novel, rapid, specific and stability-indicating reverse-phase high-performance liquid chromatography method was developed for the quantitative determination of related compounds, obtained from two different synthetic routes and degradation products of Azilsartan kamedoxomil (AZL). The method was developed by using a YMC-Pack pro C18 (150 × 4.6 mm, 3 µm) column with a mobile phase containing a gradient mobile phase combination. The eluted compounds were measured at wavelength 220 nm. The developed method run time was 25 min, within which AZL and its eight impurities were well separated with minimum 3.0 resolution. The drug substance was subjected to stress conditions of hydrolysis (acid, base and water), oxidation, photolysis, sunlight, 75% relative humidity and thermal degradation as per International Conference on Harmonization (ICH) prescribed stress conditions to ascertain the stability-indicating power of the method. Significant degradation was observed during acid, base, peroxide, water hydrolysis and 75% relative humidity studies. The mass balance of AZL was close to 100% in all the stress condition. The developed method was validated as per the ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness.

Quality Control Assay of Two Antihypertensive Representatives Using Rp-HPLC Based Methodology: Stress Assessment on Antihypertensive Representatives

“…Shrinivasan et al [11] Masthanamma and Jahnavi [12], Sreenivasulu [13] proposed RP-HPLC [11,12] and LC-MS [13] for quantification of AZIL drug alone in in bulk and formulations tablets. Sohni et al [14], Naazneen and Sridevi [15], Aher et al [16] Rao et al [22] and Sawaikar and Kapupara [23].…”

Simultaneous Estimation of Azilsartan and Cilnidipine in Bulk by Rp-HPLC and Assessment of Its Applicability in Marketed Tablet Dosage Form

“…Extensive literature research revealed some analytical methods for the estimation of Azilsartan medoxomil by RP-HPLC alone [13,14]. Further, Sreenivasulu J et al reported the estimation of related compounds in Azilsartan medoxomil using LC-MS [15]. Chandana et al recently reported stability-indicating the RP-HPLC method for the estimation of Azilsartan medoxomil and its related substances.…”

The Development and Validation of Fast and Robust Stability Indicating RP-HPLC Method for Simultaneous Estimation of Azilsartan Medoxomil and Cilnidipine in Pharmaceutical Dosage Form

“…3 It is reported officially in Indian Pharmacopoeia (IP)-2018. 4 Literature study revealed that the analytical techniques like HPTLC, [5][6] HPLC, [7][8] UVspectrophotometry, 9,10 LC/MS-MS [11][12] methods have been presented for determination of Azilsartan medoxomil and Cilnidipine as a single, while for the combination of Azilsartan medoxomil and Cilnidipine method is available on UV-spectroscopy 13 and HPLC, 14 there is no article related to Stability Indicating HPLC Assay method to quantify Azilsartan medoxomil and Cilnidipine in bulk has ever been mentioned within literature referred. The primary goal of this project was to produce a specific, accurate, and reproducible stability indicating HPLC methods for determination of Azilsartan medoxomil and Cilnidipine as stated in the ICH guidelines.…”