Simultaneous Estimation Of Metformin Research Articles

Stability Indicating HPLC Method Development and Validation for Simultaneous Estimation of Metformin and Empagliflozin in Bulk and Pharmaceutical Dosage Form

In the present work, simple, accurate and rapid stability indicating RP-HPLC method has been developed for the simultaneous estimation of Metformin and Empagliflozin in bulk and tablet dosage form. Separation of analytes was carried out on Ascentis C18 HPLC column (4.6 x 150 mm, 5 μm) using a mobile phase of 0.1% orthophosphoric acid and acetonitrile (60:40, v/v), at a flow rate of 1.0mL/min and measurement carried out at UV 260 nm. The validation parameters namely linearity, sensitivity, selectivity, specificity. robustness, precision and accuracy were determined. The peak area response-concentration curve was linear, over the concentration range of 125-750 μg/mL for Metformin and 1.25-7.50 μg/mL for Empagliflozin with quantitation limits of 4.59 μg/mL for Metformin, and 0.08 μg/mL for Empagliflozin. The proposed method was successfully validated for the determination of Metformin and Empagliflozin simultaneously in combined tablet dosage form. The performance of the present method was compared with available RP-HPLC methods and found to be rapid and economical. The proposed stability-indicating RP-HPLC method can be successfully applied to quality control and drug analysis.

DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING SIMULTANEOUS ESTIMATION OF METFORMIN AND ALOGLIPTIN IN TABLETS BY HIGH-PERFORMANCE THIN LAYER CHROMATOGRAPHY

Objective: A simple and stability-indicating high-performance thin-layer chromatographic method was developed and validated for the simultaneous estimation of metformin and alogliptin in tablets.
 Methods: The method was developed in TLC aluminum plates pre-coated with silica gel 60F254 as the stationary phase and the solvent system consists of methanol: chloroform: 0.5% ammonium sulphate [4:4:2, v/v/v]. The system was found to conferred a compact spot for metformin [Rf value of 0.44±0.02] and alogliptin [Rf value of 0.66 ± 0.22]. Densitometric analysis of metformin and alogliptin was carried out at the wavelength of 254 nm. Forced degradation studies were conducted to know the stability of the drug samples under various stress conditions like acid, base, peroxide, photolytic degradation according to the ICH guidelines.
 Results: The developed method was found to be suitable for the excellent separation of the drug samples. Calibration curves were linear in the range of 40-200 ng/spot with a correlation coefficient of 0.996 for metformin and calibration curves were linear in the range of 1-5 ng/spot with a correlation co-efficient of 0.997 for alogliptin, respectively. Stability study shows that the chromatograms of samples degraded with acid, base, hydrogen peroxide, dry heat, and photolytic showed well-separated spots of pure metformin and alogliptin as well as some additional peaks at different Rf values. The method was successively applied to pharmaceutical formulation. No chromatographic interference from the tablet excipients was found.
 Conclusion: The newly developed method can be applied for the identification and quantitative determination of metformin and alogliptin in the combined dosage form.

STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION OF METFORMIN AND ERTUGLIFLOZIN BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY WITH PDA DETECTION AND ITS APPLICATION TO TABLET DOSAGE FORM

Objective: A sensitive, rapid, accurate, and precise stability indicating high-performance liquid chromatography method was developed and validated for the simultaneous estimation of metformin (MET) and ertugliflozin (ERT).
 Methods: The planned chromatographic method was developed using Kromasil C18 column using 0.1 M sodium dihydrogen phosphate methanol (50:50, by volume, pH 4.0) as mobile phase system followed by peak area response measurement at 238 nm. The developed method was validated by means of ICH guidelines about system suitability, linearity, sensitivity, selectivity, accuracy, precision, robustness, and specificity.
 Results: Calibration curves of MET and ERT are linear from 250 to 750 μg/ml and 3.75 to 11.25 μg/ml, respectively. Relative standard deviation is <2.0% and recovery is ̴ 100%. Successfully, the developed method was applied for the simultaneous determination of MET and ERT in tablets and to study degradation of MET and ERT in acidic, alkaline, oxidation, thermal, and photolytic degradation conditions. No obstructions from additional common excipients of tablets and degradants were observed.
 Conclusion: The results recommended method suitability for the analysis of MET and ERT in quality control laboratories.

METHOD DEVELOPMENT AND VALIDATION OF A REVERSED-PHASE LIQUID CHROMATOGRAPHIC METHOD FOR THE SIMULTANEOUS ESTIMATION OF SELECTED ANTIDIABETIC DRUGS IN THE PRESENCE OF THEIR DEGRADATION PRODUCTS

Objective: This study was designed to conduct forced degradation and validation studies for the simultaneous estimation of metformin, sitagliptin, pioglitazone, and glimepiride. Methods: Analytes were separated on an Agilent XDB-C18, 150 × 4.6 mm, 5 μm column using an isocratic elution mode having mobile phase composition of 20 mM potassium dihydrogen phosphate buffer (pH 4.0):acetonitrile (65:35% v/v). Analytes were detected at a wavelength of 225 nm. The optimized method was validated as per the ICH Q2 guidelines. Results: The retention times of metformin, sitagliptin, pioglitazone, and glimepiride were 3.47, 4.83, 5.83, and 9.44 min, respectively. The linearity was 25–100 μg/ml for metformin, 2.5–10 μg/ml for sitagliptin, 1–4 μg/ml for pioglitazone, and 0.75–3 μg/ml for glimepiride. The correlation coefficient for calibration curves was >0.99, and accuracy was between 98 and 102% for each analyte. Inter- and intra-day precisions were calculated <2% relative standard deviation for each analyte. Conclusion: A significant degradation was observed in the presence of acidic, basic, neutral, oxidative, and photolytic stress conditions. The method is simple, precise, accurate, robust, and reproducible and was able to successfully separate and quantify metformin, sitagliptin, pioglitazone, and glimepiride in the presence of their degradation products.

A NOVEL STABILITY-INDICATING REVERSE PHASE LIQUID CHROMATOGRAPHIC METHOD FOR THE SIMULTANEOUS ESTIMATION OF METFORMIN AND TENELIGLIPTIN IN PURE AND PHARMACEUTICAL FORMULATIONS

Objective: The present method was proposed to develop a simple, sensitive, rapid, accurate and stability-indicating reverse phase-high performance liquid chromatographic (RP-HPLC) method for the simultaneous estimation of metformin and teneligliptin in pure and pharmaceutical formulations. Methods: The chromatographic separation was done on Discovery [250 mm X 4.6 mm: 5 μm is particle size] using a mobile phase composed of 0.1% orthophosphoric acid buffer: acetonitrile [65:35, v/v], the flow rate is 1 ml/min and the detection was carried out with a photodiode array (PDA) at 260 nm.Results: The retention time of metformin and teneligliptin were found to be 2.517 min and 3.687 min, respectively. Stability indicating studies were conducted under the guidelines of an international conference on harmonization [ICH] Q1A R2 and the developed method was validated as per the guidelines of ICH Q2 R1. The linearity was found in the range of concentration of 125-750 μg/ml and 5-30 μg/ml for metformin and teneligliptin. The lower limit of detection (LOD) and lower limit of quantification (LOQ) was found to be 0.02μg/ml and 0.07 μg/ml for metformin and 0.19 μg/ml and 0.56 μg/ml for teneligliptin, respectively.Conclusion: A novel stability-indicating reverse phase liquid chromatographic method developed for the simultaneous estimation of metformin and teneligliptin. The proposed method was adopted for the routine estimation of metformin and teneligliptin in bulk and pharmaceutical dosage forms.

A NOVEL STABILITY-INDICATING REVERSE PHASE LIQUID CHROMATOGRAPHIC METHOD FOR THE SIMULTANEOUS ESTIMATION OF METFORMIN AND TENELIGLIPTIN IN PURE AND PHARMACEUTICAL FORMULATIONS

Objective: The present method was proposed to develop a simple, sensitive, rapid, accurate and stability-indicating reverse phase liquid chromatographic method for the simultaneous estimation of metformin and teneligliptin in pure and pharmaceutical formulations. Methods: The chromatographic separation was done on Discovery [250 mm X 4.6 mm: 5 μm is particle size] using a mobile phase composed of 0.1% orthophosphoric acid buffer: acetonitrile [65:35, v/v], the flow rate is 1 ml/min and the detection was carried out at 260 nm.Results: The retention time of metformin and teneligliptin were found to be 2.517 min and 3.687 min, respectively. Stability indicating studies were conducting under the guidelines of an international conference on harmonization [ICH] Q1A R2 and the developed method was validated as per guidelines of ICH Q2 RI. The linearity was found in the range of concentration of 125-750 μg/ml and 5-30 μg/ml for metformin and teneligliptin. The detection of limit and quantification of limit was found to be 0.02 μg/ml and 0.07 μg/ml for metformin and 0.19 μg/ml and 0.56 μg/ml for teneligliptin, respectively.Conclusion: A novel stability-indicating reverse-phase liquid chromatographic method for the simultaneous estimation of metformin and teneligliptin. The proposed method was adopted for the routine estimation of metformin and teneligliptin in bulk and pharmaceutical dosage forms.

Development and Validation of Stability Indicating Assay Method for Simultaneous Estimation of Glibenclamide and Metformin

A high performance reverse phase liquid chromatographic procedure is developed for simultaneous estimation of Metformin and Glibenclamide in combined tablet dosage form. The method was carried out on Agilent Hypersil ODS (4.6 x 250 mm) column with a mobile phase used consisting of Methanol: Water (0.1 % OPA) OPA= Ortho Phosphoric acid (80:20) and the pH of buffer was adjusted to 3 using 2M Orthophosphoric acid. The detection of the combined dosage form was carried out at 228 nm and a flow rate employed was 1 ml/min and column oven temperature at 300C. The retention times of Metformin andGlibenclamide were 3.4667 and 7.3500 minutes respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification as per ICH norms. The proposed method can be used for the estimation of these combined drugs.

Analytical Method Development and Validation of Metformin, Losartan and Glimepiride in Bulk and Combined Tablet Dosage form by Gradient RP-HPLC

Purpose : A simple, sensitive, linear, precise, and accurate method by gradient reversed-phase-high performance liquid chromatography for the simultaneous estimation of metformin (MET), losartan (LOS) and glimepiride (GLI) in bulk and in their combined tablet dosage form was developed and validated. Methodology : The separation of the three drugs was based on the use of Luna c18 (250 ~ 4.6 mm, i.e. 5 ƒEm) column in a gradient mode. Mobile phase consisted of Methanol (solvent A) and 0.1% Orthophosphoric acid [OPA] (solvent B) was set with gradient programming for 18 min and was delivered at 1 ml/min flow rate and effluents are achieved with variable wavelength: Photodiode array detector at 284 nm. The retention times of MET, LOS and GLI were found to be 3.11, 7.12 and 13.52mins respectively. The percentage assay of MET, LOS and GLI was found to be 100.5%, 100.5 and 100.4%, respectively. Calibration curves were linear for MET, LOS and GLI at concentration ranges of 30- 450 ng/ml, and 15-225ng/ml and 1-18ng/ml with the regression coefficient of 0.999 for all the three drugs and precise with (% RSD <2). The drug was subjected to various stress conditions of acid and base hydrolysis, oxidation, photolysis, thermal degradation and condition. Findings : Considerable degradation was found under all stress conditions and the degradation products were well resolved from Metformin (MET),Llosartan (LOS) and Glimepiride (GLI) in the proposed gradient RP-HPLC method. Conclusion : The method was validated by determining its linearity, accuracy, precision, system suitability and can be employed for routine quality control analysis.

Validated RP-HPLC method development for the simultaneous estimation of metformin and glimepiride in combine tablet dosage form

A force degradation profile of Metformin Hcl & Glimepiride in combine tablet dosage form on RP-HPLC was developed using Grace RP-C18 (4.6 x 150 mm, 5 m) in an gradient mode with mobile phase comprising of Acetonitrile: Dihydrogen Pott.Phosphate (pH 2.5 using 0.1% OPA) The flow rate was 0.7 mL/ min and effluent was monitored at 242 nm.. The retention times were found to be 2.06 min for MET and 5.80 min for GLIM. The assay shows a linear dynamic range of 250- 1250 g/mL for MET and 1.0-5.0 g/mL for GLIM. The calibration curves were linear (r 2 = 0.999 for MET and r 2 = 0.998 for GLIM) over the entire linear range. Mean % recovery was found to be 99.80 % for MET and 98.93 % for GLIM with % RSD was NMT 2 for both estimations which fully agrees with system suitability which is in good agreement with labeled amount of formulation. The % RSD for Intra- Day & Inter-Day Precision was NMT than 2 for both the drugs. The developed method was validated as per ICH guidelines

HPLC method development and validation for simultaneous estimation of Metformin and Piperine

HPLC method development and validation for simultaneous estimation of Metformin and Piperine

New Validated Stability Indicating RP-HPLC Method for Simultaneous Estimation of Metformin and Alogliptin in Human Plasma

A validated new stability indicating RP-HPLC method for the quantitative determination of metformin and alogliptin in human plasma was developed as per US-FDA guidelines. The drug was spiked in the plasma and extracted with mobile phase by precipitation method. The extracted analyte was injected into X-Terra C18 (4.6 × 150 mm, 3.5 μm, Make: ACE) or equivalent, maintained at 25°C temperature and effluent was monitored at 235 nm. The mobile phase was consisted of sodium dihydrogen ortho phosphate [pH 4.0]:acetonitrile [HPLC Grade] (70:30 v/v). The flow rate was maintained at 1.0 mL/min. The calibration curve for metformin and alogliptin was linear from 300.0 to 700.0 μg/mL (r2=0.997) and 7.5 to 17.5 μg/mL (r2=0.998) respectively. The inter-day and intra-day precision was found to be within limits. The Lower limit of quantification (LLOQ) for metformin and alogliptin were 5.936 and 1.983 μg/mL respectively. The average % recovery for metformin and alogliptin were 100.17 and 99.40-99.55% respectively and reproducibility was found to be satisfactory. This RP-HPLC method is suitable for determining the concentration of metformin and alogliptin in human plasma and it can applied for routine analysis for determination of the metformin and alogliptin from dosage form during pharmacokinetic study.

METHOD DEVELOPMENT AND VALIDATION OF METFORMIN, GLIMEPIRIDE AND PIOGLITAZONE IN TABLET DOSAGE FORM BY RP-HPLC

A rapid RP - HPLC method was developed and validated f or simultaneous estimation of metformin, glimepiride and pioglitazone from pharmaceutical dosage forms. A sensitive chromatographic separation was accomplished on C 18 column (100 × 4.6 mm, 5 µ) with mobile phase consisting of Methanol: phosphate buffer (p H 3.6 adjusted with ortho phosphoric acid) in the ratio of 75:25 v/v, at a flow rate of 1.0 ml / min and monitored at 238 nm. The developed method was validated in terms of accuracy, precision, linearity and limit of detection, limit of quantification, robu stness and solution stability. The proposed method can be used for the routine estimation of these drugs in combined pharmaceutical dosage forms.

Simultaneous Estimation of Metformin and Glimipride by Ultraviolet Spectrophotometry.

Simultaneous Estimation of Metformin and Glimipride by Ultraviolet Spectrophotometry.

SIMULTANEOUS DETERMINATION OF METFORMIN HYDROCHLORIDE IN ITS MULTICOMPONENT DOSAGE FORMS WITH SULFONYL UREAS LIKE GLICLAZIDE AND GLIMEPIRIDE USING HPTLC

A simple, precise, and accurate high performance thin layer chromatography (HPTLC) method was developed for the simultaneous estimation of metformin with sulfonylureas like gliclazide and glimepiride present in multicomponent dosage forms. This employs a precoated silica gel 60 F254 (0.2 mm thickness) on aluminum sheets and a mobile phase ammonium sulfate (0.25%): methanol:ethyl acetate in the ratio of 10.0:2.5:2.5 (v/v/v), having chamber saturation for 30 min at room temperature. The developing chamber was run upto 8 cm. Validation of the developed HPTLC method was carried out. Good sensitivity for all analytes was observed with UV detection. The method allowed quantitation over the 100–500 ng mL−1 range for gliclazide and 1000–5000 ng · mL−1 range for metformin hydrochloride in combination I and 300–500 ng mL−1 range for glimepiride and 150000–250000 ng · mL−1 range for metformin in combination II. The method has been applied, without any interference from excipients or endogenous substances, for the simultaneous determination of these two combinations in tablets.

Simultaneous estimation of metformin and pioglitazone by ultraviolet spectrophotometry

This work deals with the simultaneous estimation of metformin hydrochloride and pioglitazone hydrochloride in a bilayered tablet dosage form, without prior separation by two techniques. The methods employed are derivative spectrophotometery and Q analysis. The absorption maxima at 231 nm and 269 nm were used for the estimation of metformin and pioglitazone, respectively. Both the drugs and their mixture obey Beer-Lamberts law at selected wavelength at given concentration range. The result of analysis has been validated statistically and recovery studies confirmed the accuracy of the proposed method. The proposed procedures are simple, rapid, require no separation steps and can be used for the routine analysis of both drugs.