A Novel UPLC Method for Simultaneous Estimation of Ertugliflozin and Sitagliptin in Bulk and Tablet Dosage Form

2021 ◽  
pp. 4859-4862
Author(s):  
Deepthi R ◽  
Gowri Sankar D
Keyword(s):  
Dosage Form ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Sodium Hydrogen Phosphate ◽  
Acquity Uplc ◽  
Tablet Dosage

Aim: The proposed study aimed to develop a novel ultra-performance liquid chromatography (UPLC) method for the estimation of Ertugliflozin and Sitagliptin in Bulk and Tablet dosage form and validate the method in accordance with the International Conference on Harmonization guidelines. Methods: The optimized conditions for the developed UPLC method are Acquity UPLC HIBRA C18 (100mm × 2.1mm, 1.8µ) column maintained at 30°C with a mobile phase consisting of Buffer (0.01N sodium hydrogen phosphate) pH adjusted to 4.0 with dil. orthophosphoric acid: Acetonitrile in the ratio of 60:40%v/v on isocratic mode at a flow rate of 0.3mL/min. Results and conclusion: The sample was detected at 220nm. The retention time for Ertugliflozin and Sitagliptin was deemed at 1.873min and 1.260min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness, and solution stability. The method obeyed Beer’s law in the concentration range of 3.75µg/mL to 22.5µg/mL for Ertugliflozin and 25µg/mL to 150µg/mL for Sitagliptin with a correlation coefficient of 0.999 for Ertugliflozin and Sitagliptin respectively. Forced degradation studies were conducted by exposing the drug solution to numerous stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was considered within the limits, indicating that the drug is stable in stressed conditions. The developed method for the estimation of Ertugliflozin and Sitagliptin can be utilized for the routine analysis of Pharmaceutical dosage form.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF CABOZANTINIB IN PHARMACEUTICAL DOSAGE FORMS BY ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (10) ◽  
pp. 238
Author(s):  
Gorja Ashok ◽  
Sumanta Mondal
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

Objective: The proposed study aimed to develop a stability-indicating ultra-performance liquid chromatography (UPLC) method for the estimation of cabozantinib in pharmaceutical dosage form and validate the method in accordance with the International Conference on Harmonization guidelines.Methods: The optimized conditions for the developed UPLC method are Acquity UPLC Hibar C18 (100 mm × 2.1 mm, 1.7 μ) column maintained at 30°C with mobile phase consisting of 0.1% orthophosphoric acid and acetonitrile in the ratio of 55:45% v/v on isocratic mode at flow rate of 0.3 mL/ min. The sample was detected at 244 nm.Results: The retention time for cabozantinib was deemed 1.3 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness, and solution stability. The method obeyed Beer’s law in the concentration range of 20 μg/mL and 120 μg/mL with correlation coefficient of 0.9997. Forced degradation studies were conducted by exposing the drug solution to numerous stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was considered within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation of cabozantinib can be utilized for the routine analysis of pharmaceutical dosage form.

scholarly journals STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF PANOBINOSTAT LACTATEIN PHARMACEUTICAL DOSAGE FORMS BY UPLC

2018 ◽  
Vol 10 (11) ◽  
pp. 60
Author(s):  
Ashok Gorja ◽  
Sumanta Mondal
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stability Indicating Method

Objective: The present study aimed to develop a stability indicating ultra-performance liquid chromatography (UPLC) method for the estimation of panobinostat lactate in pharmaceutical dosage form and validate the method in accordance with ICH guidelines.Methods: The optimized conditions for the developed UPLC method are acquity UPLC hibar C18 (100 mm × 2.1 mm, 1.8µ) column maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 50:50%v/v on isocratic mode at flow rate 0.3 ml/min. The sample was detected at 266 nm.Results: The retention time for panobinostat was found to be 1.6 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability. The method obeyed Beer’s law in the concentration range of 50µg/ml and 300µg/ml with correlation coefficient of 0.9998. Forced degradation studies were conducted by exposing the drug solution to various stress conditions such as acidic, basic, peroxide, neutral, photolytic and thermal conditions. The net degradation was found to be within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation ofpanobinostat can be utilized for the routine analysis of pharmaceutical dosage form.

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 Stability indicating Ultra Performance Liquid Chromatography method development and validation for simultaneous estimation of artemether and lumefantrine in bulk and pharmaceutical dosage form

2019 ◽  
Vol 9 (2) ◽  
pp. 217-221
Author(s):  
Bandari Sukanya ◽  
V Mohan Goud ◽  
P Anitha
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Method Development ◽  
Ultra Performance Liquid Chromatography ◽  
Simultaneous Estimation ◽  
Regression Equations ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatography Method ◽  
Tablet Dosage

Ultra performance liquid chromatography method was developed for the simultaneous estimation of the Artemether (AMT) and Lumefantrine (LFT) in Tablet dosage form. Chromatogram was run through X-bridge C18 100 x 2.1 mm, 3.5m. Mobile phase containing Buffer 0.01N KH2PO4 (3.5pH): Acetonitrile taken in the ratio 55:45 was pumped through column at a flow rate of 0.3ml/min. Buffer used in this method was 0.01N KH2PO4. Temperature was maintained at 30°C. Optimized wavelength selected was 215nm. Retention time of AMT and LFT were found to be 0.787 min and 1.572min. %RSD of the AMT and LFT were and found to be 0.7 and 0.6 respectively. %Recovery was obtained as 99.49% and 100.22% for AMT and LFT respectively. LOD, LOQ values obtained from regression equations of AMT and LFT were 0.03, 0.08 and 0.095, 0.288 respectively. Regression equation of AMT is y = 19308x + 1509 and y = 36919x + 11566 of LFT. The developed method was simple and economical that can be adopted in regular Quality control test in Industries. Keywords: Artemether (AMT), Lumefantrine (LFT), Acetonitrile, UPLC.

Development and Validation of new RP-HPLC Method for simultaneous Estimation of Methylcobalamin, Epalrestat and Pregabalin in bulk and Pharmaceutical dosage form

2021 ◽  
pp. 5097-5100
Author(s):  
Krishnaphanisri Ponnekanti ◽  
Sunitha K. ◽  
Ganapaty S.
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Thermal Conditions ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Phase Water ◽  
The Stability

A new rapid, accurate, precise and economical reverse phase high performance liquid chromatographic method has been developed and validated for simultaneous estimation of Methylcobalamin, Epalrestat and Pregabalin in bulk and pharmaceutical dosage form. The separation was accomplished utilizing Agilent C18, 150 x 4.6mm, 5 column at a detection wavelength of 210nm utilizing the mobile phase water and acetonitrile 60: 40 v/v at the flow rate of 0.8ml/min and injection volume of 10µl. The total run time was 6.0 min. Validation discovered the method was specific, rapid, accurate, precise, reliable and reproducible. The calibration curve was linear over the concentration range of 0.37 – 2.25μg/ml of Methylcobalamin, 37.5-225μg/ml of Epalrestat and 37.5-225μg/ml of Pregabalin respectively with correlation coefficient of 0.999. The accuracy was determined by recovery studies and was found to be 99.5-100%. The precision of the results stated that the %RSD was <2%. The limits of detection for Methylcobalamin, Epalrestat and Pregabalin were 0.2, 0.9 and 1.2μg/ml, while the limits of quantification were 0.5, 1.5 and 0.9μg/ml respectively. Forced degradation study was carried out under acidic, alkaline, oxidative, photolytic and thermal conditions to prove the stability-indicating ability of the developed HPLC method. The high recovery confirms the suitability of developed method and can be further used in routine analysis.

scholarly journals Stability-indicating RP-HPLC method development and validation for simultaneous estimation of telmisartan and rosuvastatin calcium in bulk and in tablet dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Rameshwar Gholve ◽  
Sanjay Pekamwar ◽  
Sailesh Wadher ◽  
Tukaram Kalyankar
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Solution Stability ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Study Results ◽  
Tablet Dosage ◽  
Rosuvastatin Calcium

Abstract Background The stability-indicating chromatographic method was developed and validated for simultaneous estimation of telmisartan and rosuvastatin calcium in bulk and in tablet dosage form. The RP-HPLC elution was carried out at 242.0 nm using column Oyster ODS3 (150 × 4.6 mm, 5 µm) isocratically, and a mobile phase containing 10 mM phosphate buffer with 1.1 g octane-1-sulfonic acid sodium salt having pH 2.5 (adjusted with 5% OPA) and acetonitrile, with a proportion of 500:500, v/v was pumped through the column maintained at ambient (about 25 °C) temperature with 1.0 mL/min flow rate. The proposed method was validated according to ICH Q2 (R1) guideline. Results Telmisartan and rosuvastatin were eluted at 2.553 min and 4.505 min, respectively. The method is linear from 99.9073 to 299.7218 µg/mL for telmisartan (R2 = 1.000) and 23.6841 – 71.0522 µg/mL for rosuvastatin (R2 = 0.999). The average recovery percentage was found 100.51, 99.76, and 99.14% for telmisartan and 99.68, 99.72, and 98.56% for rosuvastatin at three different levels. Results of method repeatability and intermediate precision were found within acceptable limits. Results of solution stability showed that mobile phase was stable for 2 days; standard and sample preparations are stable for 1 day at room temperature as well as in the refrigerator (2–8 °C). Also, forced degradation study results show that method is stability indicating as capable of distinguishing the active analytes peak from the degraded product. Conclusion The developed stability-indicating method is linear in studied concentration range as well as precise, accurate, specific, and robust. Hence, successfully this method can be used for routine analysis and stability study. Graphical abstract

DEVELOPMENT OF STABILITY INDICATING RP-HPLC-PDA METHOD FOR THE SIMULTANEOUS ANALYSIS OF NAPROXEN SODIUM AND DIPHENHYDRAMINE HYDROCHLORIDE IN BULK AND TABLET DOSAGE FORMS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (09) ◽  
pp. 40-47
Author(s):  
B. N Nalluri ◽  
◽  
B. Mrudula ◽  
K Chitralatha ◽  
S. A Sultana ◽  
...  
Keyword(s):  
Naproxen Sodium ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Diphenhydramine Hydrochloride ◽  
Rp Hplc ◽  
The Stability ◽  
Tablet Dosage ◽  
Liquid Chromatographic

The present paper describes a sensitive and simple RP-HPLC-PDA method for the simultaneous estimation of Naproxen Sodium (NPX) and Diphenhydramine Hydrochloride (DPH) in the presence of their degradants. The drugs were subjected to stress conditions (forced degradation) to show the stability-indicating power of the method. The separation was achieved on Inertsil ODS C18 column (250×4.6mm, 5μ). The optimized liquid chromatographic conditions were found to be a mobile phase of 15mM ammonium acetate buffer: acetonitrile (60:40V/V) combination at a flow rate of 1.0 mL/min in isocratic mode with an injection volume of 10µL. The proposed method provided retention times of 4.6 and 10.8min, with linear responses over a range of 60-140μg/mL and 10-30μg/mL and regression coefficient (R2) of 0.999 and 0.996 respectively for NPX and DPH. No interference from other components of pharmaceutical dosage form and degradants was observed. The method was validated as per ICH guidelines and was successfully applied for the simultaneous estimation of both the drugs in bulk and tablet preparations.

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

SIMULTANEOUS ESTIMATION OF AMLODIPINE BESYLATE AND INDAPAMIDE BY DUAL WAVELENGTH SPECTROPHOTOMETRIC METHOD FOR COMBINED PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (04) ◽  
pp. 50-54
Author(s):  
M. P Patel ◽  
◽  
M. R Patel ◽  
R Hasumati ◽  
M. N Noolvi ◽  
...  
Keyword(s):  
Spectrophotometric Method ◽  
Dosage Form ◽  
Dual Wavelength ◽  
Simultaneous Estimation ◽  
Uv Spectrophotometry ◽  
Amlodipine Besylate ◽  
Pharmaceutical Dosage Form ◽  
First Order ◽  
Absorbance Difference ◽  
Tablet Dosage

A simple, accurate, precise, rapid, economical UV spectrophotometry method, dual wavelength spectrophotometry, has been developed and validated for estimation of Indapamide (IND) and Amlodipine besylate (AML) in combined tablet dosage form and can be used in routine analysis. In this method, the absorbance at 360 nm and 256 nm of AML were same and no interference of IND at 360 nm. was observed. So, absorbance difference at 256-360 is used for estimation of IND and absorbance at 360 nm used for AML. The method was found to be linear in the concentration range of 3-18 μg/mL for IND (r2>0.99962) and 10-60 μg/mL for AML (r2>0.99969). Mean assay was found to be 99.32% and 101.34% for IND and AML respectively. In first order derivative spectrophotometry, the absorbance at 237.4 nm (ZCP of AML) and 241 nm (ZCP of IND) were used for estimation of IND and AML respectively. The method was found to be linear in the concentration range of 1.5-9 μg/mL for IND(r2=0.99983) and 5-30 μg/mL for AML(r2=0.99966). Mean assay was found to be 99.72% and 100.28% for IND and AML respectively.

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