Degradation Studies
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K. Athulya Damodharan ◽  
. Nuaman ◽  
M. Archana ◽  
Mariya Palathingal ◽  
P. Ashisha ◽  

A simple, Precise, Accurate method was developed for the estimation of Cenobamate   by RP-HPLC technique. Chromatographic conditions used are stationary phase symmetry C18 (150 mm* 4.6 mm 5 µm), mobile phase Acetonitrile: 0.01NKH2PO4in the ratio of 55:45 and flow rate was maintained at 1.0ml/min, detection wave length was 272.0 nm; column temperature was set to 30oC. Retention time was found to be 2.908 min. System suitability parameters were studied by injecting the standard six times and results were well under the acceptance criteria. Linearity study was carried out between 25% to150 % levels, R2 value was found to be as 0.999.Precision was found to be 0.5 for repeatability and 0.8 for intermediate precision. LOD and LOQ are 0.01µg/ml and 0.03µg/ml respectively. By using above method assay of marketed formulation was carried out 100.32% was present. Degradation studies of Cenobamate were done, in all conditions purity threshold was more than purity angle and within the acceptable range.

Deepika Yadav ◽  
Satish K. Awasthi

A. J. Giri ◽  
Anjali D Kingre ◽  
J. K. Dhumal ◽  
P. R. Doifode ◽  
Pratiksha Jaybhaye ◽  

In present study, Accouring to specification of Indian pharmacopeia the content official limit of not less than (98.5%) and not more than (101.0%) of the lable amount our hypothesis was that when all different brands of metformin were expose to the different degradation parameters. The Forced degradation studies show the chemical behavior of the molecule which in turn helps in the development of formulation and package. A forced degradation study is an essential step in the design of a regulatory compliant stability program for both drug substances and products, and formalized as a regulatory requirement in ICH Guideline Q1A in 1993. Forced degradation is a degradation of new drug substance and drug product at conditions more severe than accelerated conditions.

Kalyani Peluri ◽  
S. Rajasekaran

Aim: The foremost purpose of this research work is to diminish the analysis time and to establish cost effective method for estimation of Vildagliptin by RP-UPLC. Study Design: UPLC based Quantification studies. Place and Duration of Study: Department of Pharmacy, Bhagwant University, Ajmer, Rajasthan, Indiabetween June 2020 and August 2020. Methodology: A simple, responsive and precised RP-UPLC method with good robustness was developed and validated as per ICH for the analysis of Vildagliptin in drug substance and separation of degradants generated by different forced degradation conditions. Productive separation of Vildagliptin was attained by the use of Luna C18 column (100x2.6mm and 1.6µm) with a mobile phase composition of 0.1% v/v Trifluoroacetic acid and Acetonitrile in 80:20 v/v, which was pumped with 0.5 ml/min flow rate. The eluted substances were examined with PDA detector at 239nm. Stressed degradation studies were performed with proposed method to determine the percentage degradation of Vildagliptin. Results: The RT of Vildagliptin was observed at 1.56 min. The developed method was validated as per ICHQ2B and proved that the method was precise, sensitive, specific and accurate.The lowest concentration of limit of detection (0.05µg/ml) and limit of quantification(0.5µg/ml) of Vildagliptin make obvious about the sensitivity of the method. The correlation coefficient found to be 0.9997 for given range of linear concentrations. The calculated average percentage recoveries of Vildagliptin in spiked solutions were found to be in the range of 99.1-100.5. The calculated % RSD was determined to be less than 2. Determination of degradation of amount of Vildagliptin by forced degradation studies representing the stability indicating nature of the proposed method. Conclusion: The developed method said to be highly sensitive, accurate, specific and robust, therefore this method has high probability to adopt in pharmaceutical industry for regular analysis of Vildagliptin.

2021 ◽  
Vol 225 ◽  
pp. 112768
Marisa A. Wirth ◽  
Lars Longwitz ◽  
Marion Kanwischer ◽  
Peter Gros ◽  
Peter Leinweber ◽  

Paladugu Venkata Naveen ◽  
Seru Ganapaty

Voriconazole is used for the treatment of variety of fungal infections caused by aspergillosis, candidiasis, coccidioidomycosis, histoplasmosis, penicilliosis etc. Voriconazole belongs to triazole class. Voriconazole is mainly used to treat certain patients who are not responding to other anti-fungal drugs. It works by slowing the growth of the fungi that cause infection. A new validated reverse phase stability indicating liquid chromatographic method has been developed for the assay of Voriconazole in presence of an internal standard (Rufinamide) tablets. Forced degradation studies were performed to define the selectivity and specificity of the method. Linearity was observed over the concentration range 1.0-100μg/mL with linear regression equation y = 0.4489x – 0.1262 (r2 = 0.9999). The LOQ and LOD were found to be 0.8934μg/mL and 0.2921μg/mL. The present stability indicating RP-UFLC method was validated as per ICH guidelines and can be useful for the assay of tablets and injections and also for the kinetic studies.

Deepthi R ◽  
Gowri Sankar D

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.


Objective: The present investigation is aimed to develop and validate, a simple, consistent and sensitive stability-indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for the determination of oral anti-diabetic drug Canagliflozin in bulk and pharmaceutical dosage form as per the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH-Q2 (R1)). Methods: The chromatographic separation was achieved by using Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) ZORBAX C18 (250 mm x 4.6 mm, 5μm particle size) with a mobile phase consisting of Acetonitrile: Water in a ratio of 53:47% v/v at a flow rate of 1 ml/min with an injection volume of 20 μl. Results: The Retention time of the drug Canagliflozin was found to be 2.36±0.05 min and detected at 214 nm UV wavelength. The linear regression equation was found to be y = 60702x–2156.2 with a correlation coefficient 0.9999. Stress degradation studies were performed by exposing the Canagliflozin into acidic, alkaline, oxidative, thermal and photolytic stress conditions with active samples withdrawn at different time intervals as per ICH guidelines. Conclusion: The proposed Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method was found to be robust, precise and specific for estimation of Canagliflozin in pharmaceutical dosage forms.

Molecules ◽  
2021 ◽  
Vol 26 (17) ◽  
pp. 5398
Yonelian Yuyun ◽  
Ponsiree Jithavech ◽  
Worathat Thitikornpong ◽  
Opa Vajragupta ◽  
Pornchai Rojsitthisak

A simple, precise, and accurate reversed-phase ultra-performance liquid chromatographic (UPLC) method was developed and validated for the determination of a mycophenolic acid-curcumin (MPA-CUR) conjugate in buffer solutions. Chromatographic separation was performed on a C18 column (2.1 × 50 mm id, 1.7 µm) with a gradient elution system of water and acetonitrile, each containing 0.1% formic acid, at a flow rate of 0.6 mL/min. The column temperature was controlled at 33 °C. The compounds were detected simultaneously at the maximum wavelengths of mycophenolic acid (MPA), 254 nm, and curcumin (CUR), or MPA-CUR, at 420 nm. The developed method was validated according to the ICH Q2(R1) guidelines. The linear calibration curves of the assay ranged from 0.10 to 25 μg/mL (r2 ≥ 0.995, 1/x2 weighting factor), with a limit of detection and a limit of quantitation of 0.04 and 0.10 μg/mL, respectively. The accuracy and precision of the developed method were 98.4–101.6%, with %CV < 2.53%. The main impurities from the specificity test were found to be MPA and CUR. Other validation parameters, including robustness and solution stability, were acceptable under the validation criteria. Forced degradation studies were conducted under hydrolytic (acidic and alkaline), oxidative, thermal, and photolytic stress conditions. MPA-CUR was well separated from MPA, CUR, and other unknown degradation products. The validated method was successfully applied in chemical kinetic studies of MPA-CUR in different buffer solutions.

Patel Seema A. ◽  
Sayyed Nazifa S. ◽  
Lajporiya Mobina I. ◽  
Manjra Mehfuza U. ◽  
Aejaz Ahmed ◽  

Aims: To develop and validate a new, simple, rapid, precise, and accurate An Eco-friendly RP-HPLC and UV-Method Development and Validation for an estimation of Tolvaptan in Bulk and Tablet dosage form followed by Forced Degradation Studies Place and Duration of the Study: The present work has been carried out at Ali-Allana College of Pharmacy, Akkalkuwa between November-2020 to April-2021. Methodology: The UV-Spectroscopic method was developed for the estimation of tolvaptan in bulk and tablet dosage form. The solvent selected for the tolvaptan UV analysis was 4% aq. SLS solution, the solution of 10µg/ml was scanned in UV region from 200-400 nm and the λmax value was determined. The RP-HPLC method was developed on Sunsil C18 150 mm x 4.6mm x 5μ column using acetonitrile: water [45:55] as mobile phase at flow rate 1.0 ml/min and UV detection at 266 nm. Results: The maximum absorbance was observed at 266 nm. The wavelength 266 nm was selected for further analysis of tolvaptan. The calibration curve was determined using drug concentrations ranging from 20-100 µgm/ml. The system suitability was performed by injecting a standard solution containing 200µg/ml of tolvaptan in six replicates. For two of them, the peak asymmetric were <1.5 and the theoretical plate number was >2000, and the %RSD of tolvaptan was less than 2. Conclusion: From the above results, it was concluded that the developed UV and RP-HPLC methods are precise and accurate and can be applied for the quantitative estimation of tolvaptan from bulk and tablet dosage forms. The method can be used for routine testing of tolvaptan by the pharmaceutical industry. Validation of the developed method was done as per International Conference on Harmonization (ICH) Q2R1 guidelines.

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