Analytical Method Development and Validation of Apixaban Using the QBD Approach With RP-HPLC Method And Its Stress Stability Studies

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Autor principal: Sayyed Tarannum*, Kuldeep Ramteke
Formato: Recurso digital
Publicado: Zenodo 2026
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author Sayyed Tarannum*, Kuldeep Ramteke
author_facet Sayyed Tarannum*, Kuldeep Ramteke
contents <p><span lang="EN-US">A robust, specific, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the quantitative determination of apixaban (APX) and its related impurities using an AQbD (Analytical Quality by Design) approach. The Analytical Target Profile (ATP) was defined to achieve a resolution greater than 1.5 between critical impurity pairs. Key chromatographic parameters, including buffer pH, organic phase composition, and column temperature, were optimized using the Design of Experiments (DoE) and risk assessment. The method employed a Zorbax RX-C18 column (250 × 4.6 mm, 5 µm), with mobile phases composed of Buffer: Acetonitrile (90:10, v/v) and Water: Acetonitrile (28:72, v/v) at pH 4.0 and 40 °C. The developed method exhibited excellent linearity (r² ≥ 0.999), precision (%RSD < 2%), and accuracy (recoveries = 98–112%), with high sensitivity (LOD = 0.02–0.03 ppm; LOQ = 0.05–0.10 ppm). Forced degradation under acidic, basic, oxidative, photolytic, and thermal conditions confirmed its stability capability. The established design space and control strategy ensured robustness and reproducibility in routine analyses. The validated method was successfully applied to the quantification of apixaban and its impurities in tablet dosage forms</span><span>.</span></p>
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spellingShingle Analytical Method Development and Validation of Apixaban Using the QBD Approach With RP-HPLC Method And Its Stress Stability Studies
Sayyed Tarannum*, Kuldeep Ramteke
Apixaban, AQbD, RP-HPLC, Forced Degradation, Stability-Indicating Method, Design of Experiments (DoE)
<p><span lang="EN-US">A robust, specific, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the quantitative determination of apixaban (APX) and its related impurities using an AQbD (Analytical Quality by Design) approach. The Analytical Target Profile (ATP) was defined to achieve a resolution greater than 1.5 between critical impurity pairs. Key chromatographic parameters, including buffer pH, organic phase composition, and column temperature, were optimized using the Design of Experiments (DoE) and risk assessment. The method employed a Zorbax RX-C18 column (250 × 4.6 mm, 5 µm), with mobile phases composed of Buffer: Acetonitrile (90:10, v/v) and Water: Acetonitrile (28:72, v/v) at pH 4.0 and 40 °C. The developed method exhibited excellent linearity (r² ≥ 0.999), precision (%RSD < 2%), and accuracy (recoveries = 98–112%), with high sensitivity (LOD = 0.02–0.03 ppm; LOQ = 0.05–0.10 ppm). Forced degradation under acidic, basic, oxidative, photolytic, and thermal conditions confirmed its stability capability. The established design space and control strategy ensured robustness and reproducibility in routine analyses. The validated method was successfully applied to the quantification of apixaban and its impurities in tablet dosage forms</span><span>.</span></p>
title Analytical Method Development and Validation of Apixaban Using the QBD Approach With RP-HPLC Method And Its Stress Stability Studies
topic Apixaban, AQbD, RP-HPLC, Forced Degradation, Stability-Indicating Method, Design of Experiments (DoE)
url https://doi.org/10.5281/zenodo.18310834