Stability‐indicating ultra performance liquid chromatography method development and validation for simultaneous estimation of metformin, linagliptin, and empagliflozin in bulk and pharmaceutical dosage form

Abstract

A rapid stability‐indicating reversed phase‐ultrapure liquid chromatography (RP‐UPLC) was developed and validated for the estimation of metformin (MET), linagliptin (LIN), and empagliflozin (EMP) combination in bulk and tablet dosage form using Kromasil C18 column (2.1 × 50 mm, 1.8 μm) as a stationary phase and a mixture solution of 40% phosphate buffer (pH = 3) and 60% acetonitrile as mobile phase at a flow rate of 0.6 mL/min. The detection was performed at 248 nm using a photodiode array detector. The linearity, sensitivity, selectivity, robustness, specificity, precision, and accuracy were determined. The peak area response–concentration curve was rectilinear over the range of 50–150 (MET), 5–15 (LIN), and 10–30 μg/mL (EMP) with quantitation limits of 0.042 (MET), 0.023 (LIN), and 0.059 μg/mL (EMP). The proposed method was successfully validated for the determination of MET, LIN, and EMP simultaneously in combined tablet dosage form. The performance of the proposed method was compared with reported RP‐UPLC methods and found to be rapid and economical. The developed and validated stability‐indicating RP‐UPLC method was appropriate for the quality control and drug analysis.

Application of experimental design in HPLC method optimization and robustness for the simultaneous determination of canagliflozin, empagliflozin, linagliptin, and metformin in tablet

“…Few other analytical methods were described for the simultaneous determination of LIG in combination with other antidiabetic agents using HPTLC (El-Kimary et al, 2016;Patel et al, 2020), UPLC/ UV (Ayoub, 2015;Vankalapati et al, 2021), and LC-MS/MS (Al Bratty et al, 2017;Rathod et al, 2020) methods, either in their pharmaceutical dosage form or in human plasma. In addition, other methods were reported for the determination of EMG either alone (Abdel-Ghany et al, 2018;Ayoub, Emam, et al, 2017;Manoel et al, 2021) or in combination with MEF Munde et al, 2020;Riaz et al, 2020).…”

Development and Validation of Dissolution Method for Linagliptin Tablets

“…The linagliptin was found to be stable at condition of 0.1 N HCl, 37°C. It has been reported to degrade by about 4.5% at stress condition of 0.1 N HCl and temperature of 60-80°C [11,12]. Thus, 0.1 N HCl at 37°C is suitable as dissolution medium since solution stability has been confirmed for 2 h under this condition.…”

New Validated Stability-Indicating Rp-HPLC Method for the Simultaneous Determination of Metformin Hydrochloride, Linagliptin and Empagliflozin in Bulk and Pharmaceutical Dosage Forms

“…An extensive literature search revealed that several analytical methods were reported for the analysis of metformin HCl, linagliptin, empagliflozin, a combination of metformin and linagliptin, a combination of metformin and empagliflozin, and a combination of linagliptin and empagliflozin using Ultraviolet spectroscopy [13][14][15][16], reverse phase high-performance liquid chromatography (RP-HPLC) [17][18][19][20][21][22][23][24][25], and ultra-performance liquid chromatography (UPLC) [26,27]. However, only a few RP_HPLC methods were reported for the simultaneous determination of metformin HCl, linagliptin, and empagliflozin in their recently approved fixed dosage combinations [28][29][30] and thus, there is a need to develop rapid, sensitive, and cost-effective stability indicating RP-HPLC method for the simultaneous estimation of metformin HCl, linagliptin and empagliflozin in fixed dosage combinations.…”