Determination of Canagliflozin, Dapagliflozin, and Empagliflozin in Pharmaceutical Solid Dosage Forms by the HPLC Method

Israa Al-Ani, Marwah Thamer Abbas Al Saadi, Noor T. Alsaadi, Rima H. Al Omari, Mohammed F. Hamad, Wael Abu Dayyih, Laura G. Vicas, Riad Awad

Abstract

This study aimed to develop a simple, sensitive, and accurate reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of canagliflozin, dapagliflozin, and empagliflozin in their combined pharmaceutical dosage form or individually. HPLC separation was achieved utilizing a Hypersil-T C18 (150 mm x 4.6 mm, 5-μm particle size) analytical or equivalent column. A mixture of 1% triethanolamine and 80% acetonitrile was used as the mobile phase at a flowrate of 1.2 ml/min. Detection was performed at 280 nm and ambient temperature. The retention times of canagliflozin, dapagliflozin, and empagliflozin were 1.854, 2.480, and 4.655 min, respectively. Linearity was obtained, ranging from 20 to 80 µg/ml for canagliflozin, dapagliflozin, and empagliflozin. The correlation coefficient for the method was greater than 0.999, indicating a strong linear relationship. The RP-HPLC method was thoroughly validated according to the ICH Q2 (R1) guidelines, and all validation parameters met the acceptance criteria. This validation demonstrated that the method's accuracy, precision, specificity, robustness, and limit of detection were within acceptable limits. Based on the successful validation and excellent method performance, this RP-HPLC method can be employed for the routine analysis of canagliflozin, dapagliflozin, and empagliflozin in raw materials or pharmaceutical dosage forms. Its simplicity, sensitivity, and accuracy make it a suitable choice for quality control and pharmaceutical research.

 

Keywords: canagliflozin; dapagliflozin; empagliflozin; high-performance liquid chromatography; validation; dosage form

 

https://doi.org/10.55463/issn.1674-2974.51.9.4


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References


ALKATHER Z., HAILAT M., AL-SHDEFAT R., and DAYYIH W. A. Development and validation of HPLC method for five gliptins in pharmaceutical dosage forms in finished marketed products. Current Pharmaceutical Analysis, 2020, 17(10): 1263–1271. https://doi.org/10.2174/1573412917999201102212635

ALHUSBAN A. A., HAMMAD A. M., and ALZAGHARI L. F. Simple HPLC method for simultaneous quantification of nicotine and cotinine levels in rat plasma after exposure to two different tobacco products. Acta Chromatographica, 2023, 35(1): 106-114. https://doi.org/10.1556/1326.2022.01054

EUROPEAN MEDICINES AGENCY. ICH guidelines, n.d. https://www.ema.europa.eu/en/human-regulatory-overview/research-and-development/scientific-guidelines/ich-guidelines

PFÜTZNER A., SCHÖNDORF T., HANEFELD M., and FORST T. High-Sensitivity C-Reactive Protein Predicts Cardiovascular Risk in Diabetic and Nondiabetic Patients: Effects of Insulin-Sensitizing Treatment with Pioglitazone. Journal of Diabetes Science and Technology, 2010, 4(3): 706–716. https://doi.org/10.1177/193229681000400326

JOHNSTON R., UTHMAN O., CUMMINS E., CLAR C., ROYLE P., COLQUITT J., TAN B. K., CLEGG A., SHANTIKUMAR S., COURT R., O’HARE J. P., MCGRANE D., HOLT T., and WAUGH N. Canagliflozin, dapagliflozin and empagliflozin monotherapy for treating type 2 diabetes: systematic review and economic evaluation. Health Technology Assessment, 2017, 21(2): 1–218. https://doi.org/10.3310/hta21020

KOBUCHI S., YANO K., ITO Y., and SAKAEDA T. A validated LC‐MS/MS method for the determination of canagliflozin, a sodium–glucose co‐transporter 2 (SGLT‐2) inhibitor, in a lower volume of rat plasma: application to pharmacokinetic studies in rats. Biomedical Chromatography, 2016, 30(10): 1549–1555. https://doi.org/10.1002/bmc.3720

ALHUSBAN A. A., & ATA S. A. Simple HPLC method for rapid quantification of nicotine content in e-cigarettes liquids. Acta Chromatographica, 2020, 33(3): 302–307. https://doi.org/10.1556/1326.2020.00832


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