Method Development, Validation by Simultaneous Estimation of Empagliflozin and Linagliptin by Rp-HPLC Method

Raut, Abhijeet N; Jawarkar, Shailesh G; Khodke, Vaibhav S; Khole, Vivek A

doi:10.7897/2277-4572.091160

Cited by 6 publications

(4 citation statements)

References 4 publications

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“…LIG was investigated using spectrophotometric and chromatographic methods in pure form, in pharmaceutical dosage form, and in biological fluids (Mai et al, 2020;Nannapaneni et al, 2016). On the contrary, several analytical methods based on spectrophotometry (Abdel-Ghany et al, 2017;Moussa et al, 2018) and chromatography (Abdel-Ghany et al, 2016;Ayoub, 2015;Bhole et al, 2017;Dayyih et al, 2021;EL Sheikh et al, 2020;Naazneen & Sridevi, 2016;Raut et al, 2020;Rizk et al, 2021) were described for the simultaneous determination of LIG and EMG. In addition, several methods were reported for the simultaneous quantitation of LIG and MEF in pure form, in pharmaceutical dosage form, or in human plasma.…”

Section: Introductionmentioning

confidence: 99%

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

Moussa

Mahrouse

Fawzy

2021

Biomedical Chromatography

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Gliflozins and gliptins represent two different pharmacological drug classes that exert different and potentially complementary glucose-lowering effect in patients with type II diabetes mellitus. A novel, selective, and sensitive HPLC method was developed for the determination of canagliflozin, empaglifozin, linagliptin, and metformin in pure form, in laboratory prepared mixtures, and in pharmaceutical dosage form. Experimental design optimization was applied by using Plackett-Burman and face-centered composite designs to achieve the best resolution with minimum experimental trials. Three significant variables affecting optimization, namely buffer pH, percentage of methanol, and percentage of acetonitrile, were studied. Chromatographic separation was achieved using an Agilent Eclipse C 8 column, and column temperature was kept at 45 C. The mobile phase was composed of dipotassium hydrogen phosphate buffer (0.05 M, adjusted to pH 6 using o-phosphoric acid):acetonitrile:methanol (50:25:25, v/v/v) at a flow rate of 1.5 mL/min. Sharp and wellresolved peaks of the cited drugs were obtained. The method was fully validated in terms of linearity, accuracy, precision, selectivity and robustness in agreement with the International Council of Harmonization (ICH) guidelines Q2 (R1). Satisfactory results were obtained by the analysis of tablets through applying the developed method. Therefore, it could be performed for the analysis of the cited drugs in quality control laboratories.

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Section: Introductionmentioning

confidence: 99%

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

Moussa

Mahrouse

Fawzy

2021

Biomedical Chromatography

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“…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.…”

Section: Fig 1: Chemical Structure Of Metformin Hclmentioning

confidence: 99%

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

UNADE

Pawar

2022

Int J App Pharm

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Objective: The purpose of the present study is to develop simple, fast, accurate, precise, and robust stability-indicating reverse phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of metformin HCl, empagliflozin, and linagliptin in their combinations. Methods: Separation was performed on Agilent Eclipse XDB-C18 (250 mm x 4.6 mm, 5 µm) column with a mobile phase consisting of 0.1 % triethylamine (pH =3) buffer and acetonitrile in the ratio 40: 60 (v/v) at a flow rate of 1 ml/min. Detection of the analytes was carried out at a wavelength of 240 nm with a photodiode array detector. The developed method was validated as per the International Conference on Harmonization (ICH) guidelines. Results: The retention time values under the optimized condition were 2.660 min, 3.586 min, and 5.412 min for metformin HCl, linagliptin, and empagliflozin, respectively. The method was linear over a concentration range of 100 µg/ml-1500 µg/ml, 0.5 µg/ml-7.5 µg/ml, and 2.5 µg/ml-37.5 µg/ml for metformin HCl,linagliptin and empagliflozin respectively. The limit of detection (LOD) of the method was found to be 4.00 µg/ml, 0.02 µg/ml, and 1.00 µg/ml for metformin HCl, linagliptin, and empagliflozin, respectively. The degradation peaks were clearly resolved from the parent drug peaks in the chromatograms of forced degradation studies. Conclusion: The validated method was successfully applied for the determination of metformin HCl, linagliptin, and empagliflozin in their combined tablet dosage forms and hence can be used for the routine quality control of the drugs in pharmaceutical bulk, and dosage forms.

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“…15 Empaglif lozin can be estimated using limited highperformance liquid chromatography (HPLC), reverse-phase high-performance liquid chromatography (RP-HPLC), and ultraviolet (UV) methods, according to a survey of the relevant published research. [16][17][18][19][20][21][22][23][24][25][26][27][28] This study was undertaken to determine the best RP-HPLC technique aimed at determining the quantity of empagliflozin in both bulks and pharmaceutical dosage forms. The recommendations laid out by ICH were used to perform the technique validation.…”

Section: Introductionmentioning

confidence: 99%

RP-HPLC Method Development and Validation for an Estimation of Empaglifl ozin from Bulk and Pharmaceutical Dosage Form

Avinash¹,

Gandhimathi²

2023

IJPQA

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The objective of a recent investigation was to develop an RP-HPLC technique for assessing empaglifl ozin in both bulks and pharmaceutical dosage forms. An Agilent Eclipse XDE C-18 (4.6 mm x 250 mm, 5.0 m particle size) column for separation, a mobile phase of 0.1 M TEA pH 5.5 corrected by methanol and OPA in a proportion of 4:96 percent v/v at a fl ow rate of 0.7 mL/minwas utilized towards achieving the desired peak resolution. Diagonal array detectors (DADs) are utilized to measure the eluent at a wavelength of 270 nm. The regression equations for empaglifl ozin in bulk were y = 58.924x-5.693 and the regression equations for empaglifl ozin in tablet dosage form were y=57.927x+5.027. The calibration curve shows that the peak size was proportionate toward the concentration. In the precision study, the % of the amount was found in the 100 to 101% range. In %accuracy, %RSD was found to be 99.18 to 99.84 for empaglifl ozin in bulk and 99.29 to 99.53 for empaglifl ozin in the tablet dosage form. The limit of detection (LoD) for empaglifl ozin was determined to be 0.309143 μg/mL, while the limit of quantitation (LoQ) was determined in the direction of 0.936798 μg/mL. Based on the fi ndings of the robustness experiments, it was determined that the method’s accuracy and specifi city remain within acceptable ranges when subjected to minor adjustments to fl ow rate, wavelength, and mobile phase. The established technique was suitable for use in quality control labs to determine the quantity of empaglifl ozin present in bulk and tablet formulation

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Method Development, Validation by Simultaneous Estimation of Empagliflozin and Linagliptin by Rp-HPLC Method

Cited by 6 publications

References 4 publications

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

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

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

RP-HPLC Method Development and Validation for an Estimation of Empaglifl ozin from Bulk and Pharmaceutical Dosage Form

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