AQbD-based stability indicating development and validation of azilsartan medoxomil and cilnidipine by UPLC method

Swarupa Bandi Sreedevi Adikay   

Open Access   

Published:  Jan 17, 2023

DOI: 10.7324/JAPS.2023.114999

This work describes a chromatographic technique for quantifying azilsartan medoxomil (AZL) and cilnidipine (CIL) in bulk and pharmaceutical formulations using quality by design (QbD). The analytical targeting profile distribution and critical analytical attributes (CAA) are incorporated with analytical QbD. Risk evaluation studies and factor screening research facilitate the identification of critical method parameters (CMPs). The application of 22 full factorial designs was used to optimize the process. Selected CMPs, such as plate number of peak 1 (R1), resolution (R2), and tailing factor of peak 2 (R3) were evaluated. Utilizing statistical data and response surface plots, the individual and interaction effects of CMP on CAA were evaluated. The significance (p ? 0.05) of the procedure parameters was shown by analysis of variance. Mobile phase-Acetonitrile and 1% triethylamine buffer (50:50 v/v), pH (2.5) adjusted with 0.1% ortho-phosphoric acid, and Waters X-Bridge C18 column, (50 × 4.6 mm, 2.5 μm), the flow rate is 0.5 ml/minute with photodiode array detector at 273 nm. According to ICH requirements, method validation and subsequent stress degradation experiments were carried out. All variables are within their bounds. The suggested method is effectively illustrated by using a QbD to perform extremely sensitive, stable, and suited for regular analysis and clinical applications.

Keyword:     QbD UPLC-PDA azilsartan medoxomil cilnidipine forced degradation


Bandi S, Adikay S. AQbD-based stability indicating develop­ment and validation of azilsartan medoxomil and cilnidipine by UPLC method. J Appl Pharm Sci, 2023.

Copyright: © The Author(s). This is an open-access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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Andhalea SM, Nikalje APG. Simultaneous estimation of azilsartan and cilnidipine in bulk by RP-HPLC and assessment of its applicability in marketed tablet dosage form. Int J App Pharm, 2022; 14(1):116-23.

Desai MM, Nikalje AAG. Quality-by-design based development and validation of stability indicating method by UPLC method for impurities of simvastatin from drug and pharmaceutical dosage form. IJPS, 2021; 83(1):110-9.

Deshmukh S, Vanjari S, Patil R. Application of design of experiment based innovative approach in method development and validation of RP-HPLC for estimation of azilsartan in bulk and pharmaceutical tablet dosage form. Indian J Pharm Educ Res, 2020; 54(3):657-66.

Ghante M, Akhade N, Gota P, Nikam A, Jagtap S, Nikam V. Development and validation of high-performance thin-layer chromatography method for simultaneous estimation of nebivolol hydrochloride and cilnidipine. Asian J Pharm Clin Res, 2019; 12(4):347-50.

ICH. ICH Harmonized Tripartide Guideline: validation of analytical procedure: text and methodology Q2 (R1). ICH, Silver Spring, MD, p 17, 2005.

Jani R, Patel S. Development and validation of spectrophotometric method for simultaneous estimation of azilsartan kamedoxomil and cilnidipine in synthetic mixture. World J Pharm Res, 2018a; 7(8):948-58.

Jani R, Patel S. Simultaneous spectrophotometric determination of azilsartan kamedoxomil and cilnidipine in the mixture. Int J Res Pharm Pharm Sci, 2018b; 3(2):86-90.

Jena BR, Panda SP, Kulandaivelu U, Alavala RR, Rao GSNK, Swain S, Ghose D, Pattnaik G, Pradhan DP. Analytical QbD-based systematic development of a novel RP-UHPLC method for quantification of albuterol sulfate in its metered dose inhaler formulations. J Res Pharm, 2021; 25(5):689-701.

Juran JM. Juran on quality by design: the new steps for planning quality into goods and services. The Free Press, New York, NY, 1992.

Kumar H, Begum A. Determination of azilsartan medoximil and chlorthalidone in tablets exposed to forced degradation by using RP-HPLC. Biomed Res, 2019; 30 (5):775-85.

Khan N, Ameeduzzafar, Ali A, Ahmad FJ. A novel validated stability-indicating HPTLC method to quantitate forskolin as a bulk drug and in a nanosuspension. Indian J Pharm Sci, 2018; 80(5):820-6.

Prajapati P, Tailor P, Shahi A, Acharya A, Shah S. Application of Taguchi OA and Box-Behnken design for the implementation of DoE-based AQbD approach to HPTLC method for simultaneous estimation of azilsartan and cilnidipine. J Chromatogr Sci, 2022; 60(5):bmac045.

Rathod R, Patil A, Shirkhedkar A. Novel NP, and RP-HPTLC in praxis for simultaneous estimation of chlorthalidone and cilnidipine in bulk and pharmaceutical formulation. J Anal Chem Lett, 2018; 8(6):862-71.

Ruhina T, Mamatha T. A novel RP HPLC method for development and validation of cilnidipine in bulk and pharmaceutical dosage form. Asian Pharm Tech, 2017; 5(14):72-81.

Solanki RV, Patel RB, Patel RK, Patel BM. Development and validation of fast and robust stability indicating RP-HPLC method for simultaneous estimation of azilsartan medoxomil and cilnidipine in pharmaceutical dosage form. Int J Pharm Investig, 2022; 12(3):293-8.

Soliman MM, Darwish MK, Abdel-Razeq SA. Determination of amlodipine besylate and azilsartan medoxomil by UHPLC, HPTLC, and spectrophotometric techniques. Int Res J Pure Appl Chem, 2019; 19(3):1- 13.

Sonawane S, Jadhav S, Rahade P, Chhajed S, Kshirsagar S. Development and validation of a stability-indicating method for estimation of chlorthalidone in bulk and tablets with the use of experimental design in forced degradation experiments. Scientifica (Cairo), 2016; 2016:9.

Surwade K, Saudagar R. UV Spectrophotometric method for the estimation of azilsartan medoxomil in bulk and pharmaceutical formulations. World J Pharm Res, 2015; 4(1):1667-72.

U. S. Food and Drug Administration. Guidance for industry: Q8 (2) pharmaceutical development. U. S. Food and Drug Administration, 2009.

Vyas R, Dediya P, Shah S, Shah D. Development and validation of HPTLC method for estimation of azilsartan medoxomil. Pharma Sci Monit, 2019; 10(1):108-17.

WHO. Guideline for the pharmacological treatment of hypertension in adults. WHO, Geneva, Switzerland, 2021.

Yu LX, Amidon G, Khan MA. Understanding pharmaceutical quality by design. AAPS Journal, 2014; 16(4):771-83. (Accessed 21 December 2012). (Accessed 23 October 2015). (Accessed March 2005).

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