Simultaneous determination of emtricitabine, tenofovir alafenamide fumarate and dolutegravir sodium by validated stability-indicating RP-HPLC-DAD method

• Published in: Annales pharmaceutiques françaises Vol. 81; no. 1; p. 94
• Main Authors: Rathod, S M, Patel, N C, Patel, P U
• Format: Journal Article
• Language: English
• Published: France 01.01.2023
• Subjects: Chromatography, High Pressure Liquid - methods; Drug Stability; Emtricitabine; Fumarates; Méthode HPLC indiquant la stabilité; Stability indicating HPLC method; Forced degradation; Emtrictabine; Estimation simultanée; Fumarate de ténofovir alafénamide; Simultaneous estimation; Dégradation forcée; Tenofovir alafenamide fumarate; Dolutegravir sodium; Dolutégravir sodique
• ISSN: 0003-4509
• DOI: 10.1016/j.pharma.2022.08.006

The purpose of this research was to develop and validate a stability-indicating RP-HPLC technique for simultaneous quantification of Emtricitabine (EMT), Tenofovir Alafenamide Fumarate (TEN), and Dolutegravir Sodium (DOL) in bulk and in their combined formulation. The developed approach was done on Exterra C18 column (150×4.6mm, 5μm) and Methanol and Buffer (comprising 0.1 (v/v) of Triethylamine and o-phosphoric acid in water, pH 2.6) as mobile phase in the proportion of 75:25 (v/v), eluted at 1mL/min. The analytes were quantified using DAD detector at 265nm. The approach was validated in accordance with the ICH guidelines. Linearity, precision, accuracy, specificity, Limit of Detection (LOD), Limit of Quantitation (LOQ), and robustness were used to validate the proposed method. Linear response was found in the range of 500-1500μg/mL for EMT, 62.5-187.5μg/mL for TEN and 125-375μg/mL for DOL. The LOD values of EMT, TEN and DOL were found 91.78μg/mL, 10.47μg/mL and 19.28μg/mL correspondingly. The LOQ values of EMT, TEN and DOL were found and 278.11μg/mL, 31.74μg/mL and 58.42μg/mL correspondingly. The assay outcomes for all drugs were observed between 99.11-100.84%. To access the method's stability indicating capabilities, the drugs were exposed to various environmental (acid, alkaline, neutral, oxidative, photolytic and thermal) conditions. The established approach was considered to be accurate, linear, precise, specific, robust and it can be utilized to analyse the drugs mentioned in its tablet.