Forced Degradation Studies of Sofosbuvir with a Developed and Validated RP-HPLC Method as per ICH Guidelines

2021 ◽  
Author(s):  
Abderrazaq Hamdache ◽  
Lamia Grib ◽  
Celia Grib ◽  
Lydia Adour ◽  
Hakim Zatout ◽  
...  
Keyword(s):  
Hplc Method ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Forced Degradation Studies ◽  
Degradation Studies

scholarly journals STABILITY INDICATING RP-HPLC ASSAY METHOD FOR ESTIMATION OF DIMETHYL FUMARATE IN BULK AND CAPSULES

2017 ◽  
Vol 9 (5) ◽  
pp. 121 ◽  
Author(s):  
Hemant K. Jain ◽  
Archana A. Gunjal
Keyword(s):  
Dimethyl Fumarate ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: To develop an accurate, simple, precise and specific stability indicating RP-HPLC method for estimation of dimethyl fumarate in bulk and capsules.Methods: An Inertsil ODS (150x4.6 mm, 5µ) column and a mobile phase containing acetonitrile: potassium dihydrogen phosphate buffer pH 6.8 (50:50% v/v) was used for this study. The flow rate was maintained at 1.0 ml/min; column temperature was fixed at 35 °C and UV detection was carried out at 210 nm. The forced degradation studies were performed and method was validated with as per ICH guidelines.Results: The retention time of dimethyl fumarate was found to be 3.3±0.02 min. The value of correlation coefficient between peak area and concentration was found to be 0.9993. The mean percent recovery of dimethyl fumarate in capsules was found in the range of 99.65 to 101.64%. The results of forced degradation studies indicated that the drug was found to be stable in basic, oxidative and thermal conditions while degraded in acidic conditions.Conclusion: It can be conducted from results that the developed HPLC method is simple, accurate, precise and specific. Results of stress testing study revealed that the method is stability indicating. Thus, this method can be used for routine analysis of dimethyl fumarate capsules and check their stability.  

scholarly journals Stability-indicating HPLC-DAD method for the determination of empagliflozin

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Shilpi Pathak ◽  
Pradeep Mishra
Keyword(s):  
Hplc Method ◽  
Coefficient Of Determination ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract Background A stability-indicating RP-HPLC method was developed and validated for the estimation of empagliflozin drug and its tablet dosage form using a DAD detector. The mobile phase consisted of methanol/acetonitrile/0.1%OPA (75:20:5). The peak was observed at 2.54 min using 222.0 nm absorption maxima. Results Calibration curve plot was found within the range of 10–50 µg/mL. The coefficient of determination (R2) was found to be 0.9990. Forced degradation studies were performed for the empagliflozin in various conditions, and the results were calculated as %RSD values and were found to be within the limits. Conclusion The method was validated as per ICH guidelines with respect to all validation parameters.

scholarly journals A Stability-Indicating RP-HPLC-UV Method for Determination and Chemical Hydrolysis Study of a Novel Naproxen Prodrug

2017 ◽  
Vol 2017 ◽  
pp. 1-10 ◽  
Author(s):  
Mohamed H. M. Hamid ◽  
Tilal Elsaman
Keyword(s):  
Oral Delivery ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Chemical Hydrolysis ◽  
Ich Guidelines ◽  
Forced Degradation Studies ◽  
The Stability ◽  
Average Retention Time

A new naproxen amide prodrug was synthesized and spectrally characterized and a simple, precise, and accurate stability-indicating RP-HPLC method was developed and validated for determination and chemical hydrolysis study of the prodrug. Forced degradation studies were conducted as per the International Conference on Harmonization (ICH) guidelines to establish the stability-indicating power of the method. Separations were performed on a C18 column (150 × 4.6 mm i.d., 5 μm p.s.). The mobile phase consisted of acetonitrile and phosphate buffer pH 4.0 in the ratio 60 : 40. The flow rate and injection volume were 1.0 mL/min and 15 μL, respectively. The peaks were monitored at 272 nm. The average retention time is 5.136 min. The linearity of the method was investigated in the range of 10–50 μg/mL and r2 was found to be larger than 0.9987. The LOD and LOQ were found to be 1.853 and 5.615 μg/mL, respectively. Results indicated that the degradants are well resolved and separated from the prodrug. Hydrolysis kinetics studies were carried out in buffer solutions (pH 1.2, 5.5 and 7.4) to establish the fate of the prodrug. The half-lives in the respective buffers were 23.5, 262, and 334 hours indicating sufficient stability to attain the goal of oral delivery.

scholarly journals Rp-Hplc Method for Estimation of Metoprolol Succinate and Olmesartan Medoxomil in Pharmaceutical Formulation with forced Degradation Studies

2019 ◽  
Vol 4 (03) ◽  
pp. 34-42
Author(s):  
T. Hemant Kumar ◽  
Samata Samantaray ◽  
D. Gowri Sankar
Keyword(s):  
Olmesartan Medoxomil ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Metoprolol Succinate ◽  
Rp Hplc ◽  
Water Ph ◽  
Forced Degradation Studies ◽  
Degradation Studies

A simple, specific, accurate, and precise RP-HPLC method was developed and validated for the simultaneous estimation of Metoprolol Succinate and Olmesartan Medoxomil in pharmaceutical formulation with forced degradation studies. The method was developed using Enable C 18G column (250 ×4.6 mm, 5 μm) with mobile phase consisting of methanol and water (pH adjusted to 3.5 with orthophosphoric acid in the ratio of 80: 20 % v/v with a flow rate of 1 mL/min. The UV detection was carried out at 240 nm. The retention time for Metoprolol Succinate and Olmesartan Medoxomil were found to be 3.986 and 6.092 min, respectively. The proposed method was validated for linearity, range, accuracy, precision, robustness, LOD, and LOQ. Linearity was observed over a concentration range 4-40 μg/mL for Metoprolol Succinate (r2 = 0.9999) and 5-60 μg/ml for Olmesartan Medoxomil (r2 = 0.9999). The % RSD for Intraday and Interday precision was found to be 0.57 and 0.68 for Metoprolol Succinate and 0.52 and 0.41 for Olmesartan Medoxomil. The LOD and LOQ were found to be 0.1143 μg/mL and 0.3565 μg/mL for Metoprolol Succinate and LOD and LOQ were found to be 0.0563 and 0.1782 μg/mL for Olmesartan Medoxomil respectively.

scholarly journals Development and Validation of RP-HPLC Assay Method for Vildagliptin Using Qbd Approach and Its Application to Forced Degradation Studies

2016 ◽  
Vol 8 (03) ◽  
Author(s):  
Meetali M. Chaphekar ◽  
Purnima Hamrapurkar
Keyword(s):  
Method Development ◽  
Accurate Determination ◽  
Interaction Effects ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

The concept of Quality by design (QbD) has recently gained importance in the area of analytical method development and involves understanding of the critical factors and their interaction effects by a desired set of experiments. So, the present work describes the development of Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method by QbD approach using Design of Experiments and subsequent validation for analysis of Vildagliptin in bulk drug and its pharmaceutical formulation. An efficient experimental design based on systematic scouting of all three key components of the RP‐HPLC method (Buffer pH, Organic Phase-% acetonitrile, Organic Modifier-Methanol) is presented. The significance and interaction effects of these parameters on the response variables (Retention time and tailing factor) were evaluated through statistical analysis tools like Analysis of Variance (ANOVA) and plots which revealed the final chromatographic conditions of the method. The developed method was validated and Forced degradation studies were also carried out in order to determine the stability-indicating nature of the method. The chromatographic separation was achieved on Jasco CrestPack RP C18 (250 × 4.6 mm, 5μ) column using Buffer (pH 6): Acetonitrile: Methanol (70:10:20 v/v) as mobile phase and detection was done using Photo-Diode Array (PDA) detector at 210 nm. The developed method of Vildagliptin is linear over a range of 5-15μg/ml having correlation coefficient R2 value as 0.999. The %RSD for precision and accuracy of the method was found to be less than 2%. Forced Degradation studies revealed that the method was found to be stability-indicating. The results showed that the proposed method is suitable for the precise and accurate determination of Vildagliptin in bulk and its formulation.

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