DEVELOPMENT AND VALIDATION OF STABILITY INDICATING METHOD FOR IPRATROPIUM BROMIDE BY USING RP-HPLC

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (02) ◽  
pp. 70-72
Author(s):  
Amol Bansode ◽  
Rohit Patil ◽  
Shubhangee Gaikwad ◽  
Pranav Shetti
Keyword(s):  
Ipratropium Bromide ◽  
Correlation Coefficients ◽  
Thermal Conditions ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Bulk Drug

A simple stability indicating RP-HPLC method was validated for determination of ipratropium bromide in the bulk drug. The drug was resolved using HPLC Column (Kromasil ODS 150 x 4.6 mm C18 column) with mobile phase of HPLC grade acetonitrile:potassium di-hydrogen phosphate buffer (60:40 V/V) at a flow rate of 1 ml/min. The retention time of ipratropium bromide was 3.7 min with UV detection at 254 nm. The method was validated with respect to linearity, sensitivity, accuracy, precision and robustness as per the International Conference on Harmonization (ICH) guidelines. The method was specific and it was observed that no interference with diluents. The linearity was established over the concentration range of 20-120 μg/ml with correlation coefficients (r2) 0.9958 for ipratropium bromide. The mean recovery was found to be in the range of 99.8% for ipratropium bromide. The % R.S.D. values for intraday precision study and inter-day study were <1.0%, confirming that the method was sufficiently precise. The drug was subjected to forced degradation under different conditions. The drug was degraded more in oxidative condition (28.89%) then alkaline condition (26.39%) then acidic condition (13.42%). There was no degradation seen under the thermal conditions.

scholarly journals Validation of Stability Indicating Method and Degradation Kinetic Study of Apremilast

2020 ◽  
Vol 10 (2) ◽  
pp. 76-85
Author(s):  
Jitesha Patel ◽  
Parin Chokshi ◽  
Rajashree Mashru
Keyword(s):  
Kinetic Study ◽  
Hplc Method ◽  
Forced Degradation ◽  
Order Kinetic ◽  
Degradation Kinetic ◽  
Degradation Study ◽  
Potassium Dihydrogen ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc

A novel stability indicating RP- HPLC method was developed for the estimation of Apremilast in bulk and marketed formulation. Separation was achieved by using Shimadzu HPLC Analytical Technologies Limited C18 (250 mm x 4.6 mm, 5µm) as stationary phase. The optimized mobile phase consist of potassium dihydrogen ortho phosphate (pH-3.2): acetonitrile in ratio of 40:60 %v/v with flow rate of 1mL/min by using methanol as diluent. Retention time of Apremilast was found to be 5.4 min which was estimated at wavelength 360nm. Linearity of Apremilast was observed in the concentration range of 50-400µg/mL with r² value of 0.9999. Assay of Apremilast tablet was found to be 99.14-100.75%. Stability indicating nature of RP- HPLC method was estimated by conducting degradation kinetic study. The forced degradation of Apremilast bulk indicate that degradation in acidic, alkali, oxidative and photolysis condition were found to be 21%, 6.5%, 25.7% and 3.9% respectively. The kinetic study of apremilast in alkali degradation followed first order kinetic study. The result indicate that the developed RP-HPLC method is suitable for estimation of Apremilast in presence of degradant product. The above method was validated as per ICH guideline. Keywords: Apremilast, RP-HPLC, Validation, Forced Degradation Study, Alkali Degradation Kinetic study

DEVELOPMENT OF A VALIDATED STABILITY-INDICATING METHOD FOR ESTIMATION OF ETHIONAMIDE IN TABLETS BY RP-HPLC AND CHARACTERIZATION OF ITS ISOLATED ALKALI DEGRADATION PRODUCT

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 20-27
Author(s):  
Sandeep S. Sonawane ◽  
◽  
Akshay S. Patil ◽  
Santosh S. Chhajed ◽  
Dimple S. Lalchandani ◽  
...  
Keyword(s):  
Degradation Product ◽  
Elevated Temperatures ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Alkali Hydrolysis

A simple, accurate, reproducible and specific stability-indicating RP-HPLC method was developed for estimation of ethionamide in tablets. Ethionamide was exposed to acid, alkali and neutral hydrolysis at elevated temperatures, to thermolytic degradation, peroxide-mediated oxidation at room temperature in dark and to photolytic degradation. The drug was found stable to thermolytic and photolytic conditions and to neutral hydrolysis. However, substantial degradation was obtained in acid and alkali hydrolysis and complete degradation in peroxide-medicated oxidation. Similar degradation behavior was observed when ethionamide tablets were exposed to the mentioned forced degradation conditions. The method showed adequate resolution of drug from its potential degradation products on C18 (250 × 4.6 mm, 5µ) column using mobile phase of methanol: water (50: 50 % V/V) at 1 mL/min. The drug and its potential degradation products were detected at 290 nm. The method was validated as per the ICH Q2(R1) guidelines. The enrichment of the alkali degradation product was performed and isolated by preparative TLC and further confirmed by NMR and IR spectroscopy.

FORCED DEGRADATION STUDIES OF TIZANIDINE HYDROCHLORIDE AND DEVELOPMENT OF VALIDATED STABILITY-INDICATING RP-HPLC METHOD

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (4) ◽  
pp. 50-55
Author(s):  
Shahbaz Rathor ◽  
Atul Sherje ◽  
Keyword(s):  
Thermal Degradation ◽  
Hplc Method ◽  
Base Hydrolysis ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Stress Studies ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Forced Degradation Studies

Simple and precise stability indicating RP-HPLC method for the quantitative determination of tizanidinehydrochloride (TZN) in pharmaceutical dosage form was developed and validated. The separation was achieved using Atlantis C18 column (250 x 4.6 mm, 5µm) at 25 °C using a mobile phase containing 20mM KH2 PO4 (pH 3.5):methanol in the ratio of 30:70 V/V at 0.8 mL/min flow rate and 315nm detection wavelength. The retention time for TZN was 3.7 min and showed linearity in the 5-40µg/mL range with R2 >0.99. The drug was subjected to acid/ base hydrolysis, oxidative and thermal degradation to establish stability indicating method. The method was validated as per ICHQ2 (R1) guidelines. The method was accurate, precise, and specific for TZN estimation. In stress studies, the drug was found to be stable to acid/alkaline hydrolysis, oxidation, and thermal degradation conditions. Thus, the reported method can be used as a stability-indicating method for quality control and routine analysis of TZN.

scholarly journals Forced Degradation of Flibanserin Bulk Drug: Development and Validation of Stability Indicating RP-HPLC Method

2022 ◽  
Vol 56 (1) ◽  
pp. 32-42
Author(s):  
Yik-Ling Chew ◽  
Hon-Kent Lee ◽  
Mei-Ann Khor ◽  
Kai-Bin Liew ◽  
Bontha Venkata Subrahmanya Lokesh ◽  
...  
Keyword(s):  
Drug Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug ◽  
Development And Validation

Development and Validation of Stability Indicating RP-HPLC Method for Determination of Enzalutamide

2019 ◽  
Vol 12 (5) ◽  
pp. 4635-4645
Author(s):  
Pankaj Padmakar Nerkar ◽  
Sameer Ansari ◽  
Shailesh Chalikwar
Keyword(s):  
Ammonium Acetate ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation

A simple, isocratic, and accurate reversed phase HPLC method was developed for the quantitative determination of enzalutamide. The chromatographic separation was achieved on an Qualisil BDS C18 (250 mm x 4.6mm, 5 μm) column using methanol: ammonium acetate buffer pH 4.2 adjusted with glacial acetic acid: (60:40, v/v) as a mobile phase, at a flow rate of 1 ml/min and detection at 236nm. The linear range for enzalutamide were 2.0 to        10 μg/mL was obtained with correlation coefficients ≥ 0.998. The retention time was found to be 6.30min. Enzalutamide was subjected to stress conditions hydrolysis (acid, base) oxidation, photolysis and thermal degradation and the stressed samples were analysed by the developed method. The method was validated for the precision, accuracy, linearity and robustness. The developed stability indicating method for enzalutamide was validated as per ICH guidelines.

scholarly journals Development of a Validated Stability Indicating Rp-Hplc Method for the Estimation of Pirfenidone in Bulk Drug and Tablet Dosage form

2021 ◽  
pp. 110-118
Author(s):  
C. Vanitha ◽  
Sravani Singirikonda
Keyword(s):  
Thermal Degradation ◽  
Dosage Form ◽  
Hplc Method ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Tablet Dosage

Objective: The present work focused on developing a validated stability indicating RP-HPLC method for the estimation of pirfenidone in bulk drug and tablet dosage form. Methods: The chromatographic separation was performed on symmetry C18 (150 mm x 4.6, 5 micron) with a 1 ml/min flow rate at 315nm. The mobile phase employed was orthophosphoric acid buffer: acetonitrile (65:35). Column temperature was maintained at 30ºC. Pirfenidone was subjected to different forced degradation conditions according to ICH guidelines, including acid, base and neutral hydrolysis, oxidation, photolysis and thermal degradation.  Results: In alkali, acidic, oxidation and UV degradation conditions the drug shows considerable degradation. Pirfenidone was stable under neutral hydrolysis and thermal degradation. Pirfenidone was stable under extreme degradation conditions showing less than 8% of degradation in all degradation conditions. This result showed that pirfenidone was stable under stress degradation. Then the optimized method was validated for the parameters like linearity, accuracy, precision and robustness as per ICH guidelines.

scholarly journals Validated Stability Indicating RP-HPLC Method for Simultaneous Estimation of Codeine Phosphate and Chlorpheniramine Maleate from Their Combined Liquid Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Ramakrishna Kommana ◽  
Praveen Basappa
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Codeine Phosphate ◽  
Chlorpheniramine Maleate ◽  
Combination Drug ◽  
Stability Indicating ◽  
Rp Hplc

The present paper describes the development of quick stability indicating RP-HPLC method for the simultaneous estimation of codeine phosphate and chlorpheniramine maleate in the presence of its degradation products, generated from forced degradation studies. The developed method separates codeine phosphate and chlorpheniramine maleate in impurities/degradation products. Codeine phosphate and chlorpheniramine maleate and their combination drug product were exposed to acid, base, oxidation, dry heat, and photolytic stress conditions, and the stressed samples were analysed by proposed method. The proposed HPLC method utilizes the Shimadzu HPLC system on a Phenomenex C18 column (, 5 μ) using a mixture of 1% o-phosphoric acid in water : acetonitrile : methanol (78 : 10 : 12) mobile phase with pH adjusted to 3.0 in an isocratic elution mode at a flow rate of 1 mL/min, at 23°C with a load of 20 μL. The detection was carried out at 254 nm. The retention time of codeine phosphate and chlorpheniramine maleate was found to be around 3.47 min and 9.45 min, respectively. The method has been validated with respect to linearity, robustness, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The developed validated stability indicating HPLC method was found to be simple, accurate, and reproducible for the determination of instability of these drugs in bulk and commercial products.

Stability Indicating Assay Method Development and Validation of Simultaneous Estimation of Chlorzoxazone, Diclofenac Sodium and Paracetamol in Bulk Drug and Tablet by RP-HPLC

2021 ◽  
pp. 5024-5028
Author(s):  
Krutika Patel ◽  
Sudheer Kumar Verriboina ◽  
S.G. Vasantharaju
Keyword(s):  
Method Development ◽  
Diclofenac Sodium ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, accurate, specific and stability-indicating RP-HPLC method was developed for simultaneous determination of chlorzoxazone, diclofenac sodium and paracetamol, using C18 Vydac Monomeric 120A (250 × 4.6mm, 5μ) at 40ºC. The mobile phase contains a mixture of 20mM potassium dihydrogen phosphate buffer (pH 6.2 adjusted with potassium hydroxide) and acetonitrile (30:70 v/v). The flow rate was 1ml/min and detection was carried out at 275nm using PDA detector. The retention time of paracetamol, chlorzoxazone and diclofenac sodium were 3.28mins, 13.27mins and 15.61mins respectively. The analytical curve was linear over a concentration range of 0.65- 6.5μg/ml for paracetamol, 1-10μg/ml for chlorzoxazone and 0.1-1μg/ml for diclofenac sodium. The drugs in bulk and tablet were subjected to acid and alkali hydrolysis, oxidation, thermal and photolytic degradation. This method can be successfully employed for simultaneous quantitative analysis of Chlorzoxazone, Diclofenac sodium and Paracetamol in bulk drug and tablet formulation.

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.  

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