scholarly journals A Stability Indicating RP-HPLC Method Validation for Simultaneous Estimation of Metformin HCl, Dapagliflozin and Saxagliptin in Pharmaceutical Dosage Form

2021 ◽  
pp. 754-767
Author(s):  
Darshak Patel ◽  
Ujashkumar Shah ◽  
Jayvadan Patel ◽  
Darshana Patel ◽  
Pavan Patel
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Metformin Hcl

Aims: Metformin HCl, Dapagliflozin and Saxagliptin is a new drug combination for the treatment of Diabetes Mellitus which is one of the oldest and lethal diseases of mankind. Aim of the research work was to develop and validate novel, rapid, sensitive, specific, robust stability indicating analytical method for simultaneous estimation of: Metformin HCl, Dapagliflozin and Saxagliptin in pharmaceutical dosage form as fixed dose formulation. Study Design: Method development and validation was performed as recommended in ICH guideline “Validation of analytical procedures: Test and Methodology Q2 (R1)”. Methodology: Method develop with chromatographic parameters as C18 column (250mm×4.6 mm, 5mm particle size), HPLC system with PDA detector and mobile phase contained a mixture of Phosphate Buffer pH 3.5 and Acetonitrile (80:20 v/v) + 1 ml triethylamine per 100 ml mobile phase. The flow rate was set to 1 ml/min with responses measured at 265 nm, injection volume was 20 µl, and run time of 15 mins. Results: The retention time of Metformin HCl, Dapagliflozin and Saxagliptin was 5.8 min, 6.8 mins and 8.4 min respectively with resolution of 3.5 between Metformin HCl and Dapagliflozin and 4.5 between Dapagliflozin and Saxagliptin. Linearity was established in the range of 250-1500 µg/ml for Metformin HCl, 1.25-7.5 µg/ml for Dapagliflozin and Saxagliptin with correlation coefficients more than 0.999. The percentage recoveries were between 98.39-101.66 for Metformin HCl, 99.01-101.77 for Dapagliflozin and 98.88-101.87 for Saxagliptin Validation parameters were evaluated according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. The forced degradation studies were performed by using HCl, NaOH, H2O2, thermal and UV Radiation. The developed method was successfully applied for the quantification and hyphenated instrumental analysis. Conclusion: Significance of developed method is that it can be utilize for routine or unknown sample analysis of assay of Metformin HCl, Dapagliflozin and Saxagliptin in pharmaceutical dosage form developed by various Pharmaceutical Industry.

scholarly journals A Stability Indicating RP-HPLC Method Validation for Simultaneous estimation of Metformin HCl and Canagliflozin in Pharmaceutical Dosage Form

2021 ◽  
pp. 180-192
Author(s):  
Darshak Patel ◽  
Ujashkumar Shah ◽  
Jayvadan Patel ◽  
Hirak Joshi ◽  
Darshana Patel ◽  
...  
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Fixed Dose ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Metformin Hcl

Aims: Canagliflozin and Metformin HCl is a new drug combination for the treatment of Diabetes Mellitus which is one of the oldest and lethal diseases of the mankind. Aim of the research work was to develop and validate novel, rapid, sensitive, specific, robust stability indicating analytical method for the simultaneous estimation of Canagliflozin and Metformin HCl in the pharmaceutical dosage form as fixed dose formulation. Study Design: Method development and validation was performed as recommended in ICH guideline “Validation of analytical procedures: Test and Methodology Q2(R1)”. Methodology: Method develop with chromatographic parameters as C18 column (250mm×4.6 mm, 5mm particle size), HPLC system with PDA detector and mobile phase contained a mixture of Phosphate Buffer pH 5.0 and Acetonitrile (60:40 v/v). The flow rate was set to 1ml/min with responses measured at 290 nm, injection volume was 20 µl, and run time of 15 mins. Results: The retention time of Metformin Hydrochloride and Canagliflozin was 5.4 min and 7.6 min respectively with resolution of 7.0. Linearity was established in the range of 10-30 µg/ml for Metformin Hydrochloride and 0.5-1.5 µg/ml for Canagliflozin with correlation coefficients more than 0.999. The percentage recoveries were between (98.62-101.22%) and (98.68-101.27%) for Metformin Hydrochloride and Canagliflozin respectively. Validation parameters were evaluated according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. The forced degradation studies were performed by using HCl, NaOH, H2O2, thermal and UV radiation. The developed method was successfully applied for the quantification and hyphenated instrumental analysis. Conclusion: Significance of developed method is that it can be utilize for routine or unknown sample analysis of assay of Metformin HCl and Canagliflozin in pharmaceutical dosage form developed by various Pharmaceutical Industry.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Midostaurin in Bulk and Pharmaceutical Dosage Form

2020 ◽  
Vol 11 (4) ◽  
pp. 5108-5112
Author(s):  
Narayanaswamy Harikrishnan ◽  
Gejalakshmi Subramanian ◽  
Hemalatha C N ◽  
Pavankumar V
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Area Measurement ◽  
Internal Diameter ◽  
Limit Values ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Hplc Method Development

An elementary, Valid, speedy and decisive strategy was developed to determine Midostaurin quantitatively in a fixed dosage form. Effective Chromatographic separation of Midostaurin was achieved by using Hypersil C18 Column (250 mm X 4.6 mm internal diameter, five μm particle size) using a mobile phase composed of Methanol and Buffer in the proportion of 75:25(by volume). The Mobile phase was siphoned using a gradient HPLC system at a flow rate of 1.0 ml/min, and quantification was based on peak area measurement at 270 nm. RT (Retention Time) for Midostaurin was 2.142 min, and dimensionality of Midostaurin was found to be linear with a statistic value of 0.999. The acceptance criteria of precision were relative variance should be less than 2.0%, and also the strategy showed precision 0.3 for Midostaurin, which shows that the tactic was precise. The full Recovery was found to be 99.96 %. Detection Limit and Quantitation Limit values for Midostaurin were found as 0.439 & 1.466. The exactness and authenticity were assessed by evaluation of validation parameters like linearity, precision, specificity, accuracy, LOD, LOQ values as per ICH guidelines. The proposed strategy has been applied to the formulation without additives interference and specific for the estimation of Midostaurin.

Development and Validation of Stability Indicating HPLC Method for the Simultaneous Estimation of LevocloperastineFendizoate and Chlorpheniramine Maleate in Pharmaceutical Dosage Form

2017 ◽  
Vol 8 (03) ◽  
Author(s):  
Sankalp Patel ◽  
Jinal Tandel ◽  
Samir Shah
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Chlorpheniramine Maleate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Stress Degradation

The aim of the present study was to develop and validate stability indicating HPLC method for simultaneous estimation of LevocloperastineFendizoate (LCP) and Chlorpheniramine Maleate (CPM). HPLC method for simultaneous analysis of both drugs was developed and validated according to ICH guideline. Efficient chromatographic separation was achieved on ODS column C18 (250 mm × 4.6 mm, 5 μm) using the optimized mobile phase. Stability indicating assay method was carried out by different stress degradation conditions. In HPLC method, the Retention time for LCP and CPM was 3.173 min and 5.060 min using optimized mobile phase Phosphate buffer (pH-3.5): Methanol (60:40 %v/v) and UV detection at 273 nm. The degradation of LCP, CPM and Formulation was shown to be highest in alkaline condition. Linearity was observed in concentration range of 20-80 μg/ml for LCP and 4-16 μg/ml for CPM. The correlation coefficient of LCP and CPM were respectively 0.9992 and 0.9994. All validation parameters were within the acceptable range. The LOD and LOQ values for HPLC method were found to be 0.146 μg/ml and 0.444 μg/ml for LCP and 0.0113 μg/ml and 0.0344 μg/ml for CPM respectively. The Method validation parameters showed %RSD value less than 2.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF SACUBITRIL AND VALSARTAN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (5) ◽  
pp. 1
Author(s):  
Shweta Mishra ◽  
C. J. Patel ◽  
M. M. Patel
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Development And Validation ◽  
Tablet Dosage

Objective: This study aims to develop and validate a stability indicating HPLC method for simultaneous estimation of sacubitril and valsartan in pharmaceutical dosage form.Methods: Sacubitril and valsartan separation were achieved by LC-20 AT C18 (250 mm x 4.6 mm) column and buffer (potassium phosphate, pH 3.0): methanol (50:50) as mobile phase, at a flow rate of 1 ml/min (millilitre per minute). Detection was carried out at 224 nm (nanometer). The different HPLC experimental parameters were optimized and the method was validated according to the standard guideline. Forced degradation experiments were carried out by exposing sacubitril and valsartan standard and sample for thermal, photolytic, oxidative and acid-base hydrolytic stress conditions.Results: Retention time of sacubitril and valsartan were found to be 4.170 min (minute) and 6.530 min (minute) respectively. The method has been validated for linearity, accuracy, precision, LOD, and LOQ. Linearity observed for sacubitril is 12.25-36.75 μg/ml (microgram per milliliter) and for valsartan is 12.75-38.25 μg/ml (microgram per milliliter). The results showed that sacubitril and valsartan and the other degradation products were fully resolved and thus the proposed method is stability-indicating.Conclusion: The proposed HPLC method was found to be simple, specific, precise, accurate, rapid and economical for simultaneous estimation of valsartan and sacubitril in bulk and tablet dosage form. Thus the validated economical method was applied for forced degradation study of sacubitril and valsartan tablet.

scholarly journals NEW STABILITY-INDICATING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF LENVATINIB MESYLATE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (9) ◽  
pp. 140
Author(s):  
Jahnavi Bandla ◽  
S. Ganapaty
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Validation Parameters ◽  
Bulk Drug

Objective: The objective of the present study was to develop and validate a new stability-indicating method for the quantification of lenvatinib mesylate in bulk drug and pharmaceutical dosage form using ultra performance liquid chromatography (UPLC).Methods: The optimized chromatographic conditions for elution of drug included UPLC HSS C18 (100 mm × 2.1 mm, 1.8 m) column, mixture of 0.1% orthophosphoric acid and acetonitrile (50:50 v/v%) mobile phase run on an isocratic mode at a flow rate of 0.3 mL/min, 240 nm detection wavelength, and column oven temperature maintained at 30°C.Results: The retention time for lenvatinib was found to be 1.24 min. The developed method was validated for various validation parameters in accordance with the International Conference on Harmonization guidelines. The method obeyed Beer’s law in the concentration range of 2.5– 15 μg/mL with a correlation coefficient of 0.9996. The percentage relative standard deviation and percentage recovery were determined to be 0.4 and 99.66–100.30%, respectively. The developed method was found to be accurate, precise, specific, linear, rugged, and robust. Forced degradation studies were conducted by exposing the drug to diverse stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was obtained within the limits.Conclusion: The developed method for the estimation of lenvatinib can be employed to routine analysis of pharmaceutical dosage form.

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