scholarly journals Analytical Separation and Characterisation of Degradation Products and the Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Levosalbutamol Respules Formulation

2017 ◽  
Vol 2 (03) ◽  
pp. 83-92
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Stress Study ◽  
The Stability ◽  
Development And Validation

A short selective, precise, accurate and sensitive stability-indicating gradient LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Levosalbutamol in pharmaceutical respules formulations. During the stress study, the degradation products of Levosalbutamol were well-resolved from Levosalbutamol and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness, and robustness. During the stability analysis of the drug product, one unknown impurity was detected by the above stability-indicating method. The flow rate was 0.8 ml/min and effluent was monitored at 242nm. Retention time was found to be 2.237±0.08 min. The LOD and LOQ values were found to be 0.20984 (μg/ml) and 0.6359 (μg/ml) respectively.

scholarly journals Analytical Separation and Characterisation of Degradation Products and the Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Ipratropium Bromide Respules Formulation

2017 ◽  
Vol 2 (03) ◽  
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Ipratropium Bromide ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Stress Study ◽  
The Stability ◽  
Development And Validation

A short selective, precise, accurate and sensitive stability-indicating gradient LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Ipratropium bromide in pharmaceutical respules formulations. During the stress study, the degradation products of Ipratropium bromide were well-resolved from Ipratropium bromide and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness, and robustness. During the stability analysis of the drug product, one unknown impurity was detected by the above stability-indicating method. The flow rate was 0.5 ml/min and effluent was monitored at 242nm. Retention time was found to be 5.0150.15 min. The LOD and LOQ values for were found to be 0.20996 (?g/ml) and 0.63624 (?g/ml) respectively.

scholarly journals Analytical Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Budesonide Respules Formulation

2017 ◽  
Vol 2 (03) ◽  
pp. 46-54
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Stress Study ◽  
Analytical Development ◽  
The Stability ◽  
Development And Validation

A short selective, precise, accurate and sensitive stability-indicating LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Budesonide in pharmaceutical respules formulations. During the stress study, the degradation products of Budesonide were well-resolved from Budesonide and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness and robustness. During the stability analysis of the drug product, all known impurities were detected by the above stability-indicating method. The flow rate was 0.8 ml/min and effluent was monitored at 247nm. Retention time was found to be 17.329±0.75 min and18.439±0.65 min of epimers (22R and 22S)respectively. The LOD and LOQ values for were found to be 0.20936 (μg/ml) and 0.6344 (μg/ml) respectively.

scholarly journals Analytical Separation and Characterisation of Degradation Products and the Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Montelukast Oral Dosage Formulation

2017 ◽  
Vol 2 (03) ◽  
pp. 69-77
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Oral Dosage ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Stress Study ◽  
The Stability ◽  
Development And Validation

A short selective, precise, accurate and sensitive stability-indicating gradient LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Montelukast in pharmaceutical oral dosage formulations. During the stress study, the degradation products of Montelukast were well-resolved from Montelukast and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness, and robustness. During the stability analysis of the drug product, one unknown impurity was detected by the above stability-indicating method. The flow rate was 0.5 ml/min and effluent was monitored at 226nm. Retention time was found to be 7.836±0.012 min. The LOD and LOQ values were found to be 0.2099 (μg/ml) and 0.6362 (μg/ml) respectively.

scholarly journals Development and Validation of Stability-Indicating GC-FID Method for the Quantitation of Memantine Hydrochloride and Its Nonchromophoric Impurities in Bulk and Pharmaceutical Dosages

2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Sanjay A. Jadhav ◽  
Shashikant B. Landge ◽  
Navanath C. Niphade ◽  
Saroj R. Bembalkar ◽  
Vijayavitthal T. Mathad
Keyword(s):  
Drug Product ◽  
High Sensitivity ◽  
Bulk Sample ◽  
Fused Silica ◽  
Stability Indicating ◽  
Flame Ionization ◽  
Stability Indicating Method ◽  
Fused Silica Capillary ◽  
The Stability ◽  
Development And Validation

A stability-indicating method has been developed and validated for the quantitative determination of memantine hydrochloride and its nonchromophoric impurities in drug substance and drug product using gas chromatography coupled with flame ionization detector (GC-FID). The stability-indicating nature of the method has been proved by establishing peak purity and confirming the mass balance of all samples by subjecting them to stress conditions like hydrolysis, oxidation, photolysis, and thermal degradation studies. The chromatographic separation was performed on a fused silica capillary (HP-5, 30 meter, 0.32 mm and 0.25 μm film thickness) column. The method validation results indicate that the method has acceptable specificity, accuracy, linearity, precision, robustness, and high sensitivity with detection limits and quantitation limits ranging from 0.001% to 0.01% and 0.004% to 0.03%, respectively. The effectiveness of the technique was demonstrated by analysis of different bulk sample of Memantine hydrochloride. The proposed GC-FID method was also found to be specific and selective for the analysis of commercial formulation samples.

Development and validation of Stability-indicating RP-UPLC Method for the Simultaneous Determination of Ivacaftor, Tezacaftor and Elexacaftor in bulk and their Formulation

2021 ◽  
Vol 25 (12) ◽  
pp. 107-115
Author(s):  
V.V.S.S.N. Raju Sri Datla ◽  
Manikandan Ayyar
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Drug Product ◽  
Dosage Forms ◽  
Combination Drug ◽  
Ultraviolet Detection ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Development And Validation

A simple reproducible stability indicating RP-UPLC method was developed for the simultaneous determination of Ivacaftor, Tezacaftor and Elexacaftor in their combined dosage forms using HSS C18, 1.8μm, 100mm x2.1 mm i.d. column. A mobile phase of phosphate buffer (10mM) pH-4.8 and acetonitrile in the ratio of 70: 30v/v mixture was used for separation and quantification of ivacaftor, tezacaftor and elexacaftor. The present drug analytes were run at a flow-rate of 0.3ml/ min at 30°C temperature. The injection volume was 2μL and with ultraviolet detection at 270nm. Under these conditions, elexacaftor, ivacaftor and tezacaftor were eluted at 0.72min, 1.4min and 1.9min respectively with a total run time shorter than 5min. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The developed RP-UPLC method was applied successfully for quality control assay of Ivacaftor, Tezacaftor and Elexacaftor in their combination drug product.

High Performance HPLC-UV Method Development and Validation for Sulfadoxine from its Potential Interfering Impurities

2021 ◽  
Vol 08 ◽  
Author(s):  
Nayan S. Gadhari ◽  
Jayram V. Gholave ◽  
Suyog S. Patil ◽  
Ajay R. Patil ◽  
Kiran F. Shelke ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Degradation Products ◽  
Drug Product ◽  
Ich Guidelines ◽  
Daunting Task ◽  
Method Development And Validation ◽  
The Stability ◽  
Development And Validation

Objective: To address the separation of interfering potential impurities associated with the drug is always a daunting task. We present the method validation and quantitative determination of sulfadoxine (SUL), an anti-malarial drug with most important interfering impurities present pharmaceutical dosages and in bulk samples using HPLC-UV method. Methods: The UV detection was obtained at 270 nm and SUL is separated on Sunfire C18 (25 cm x 4.6 mm x 5 µ m) column at 45°C with flow rate of 1.0 mL/min in a mobile phase (CH3COOH:CH3CN). The stress testing (acidic/basic/oxidative) was performed using HPLC for SUL and its impurities showing the highly efficient separation peaks between degradant and drug product. Results: The developed method was found to be highly accurate and sensitive in regulation with ICH guidelines. Also, it was found to be free from interference from degradation products which allows the stability indicating capability of developed HPLC-UV method for SUL for validation in bulk drugs. Conclusion: The main advantages of the present method; (a) Separation achieved in 30 minutes, (b) MS compatible mobile phase renders this developed method can be directly adapted to LC-MS without any major modifications in near future, and (c) separation of twelve impurities on Sunfire C18 column. The CFs (correction factors) had been calculated for all the impurities. It was found to be 1.6 (IMP IX), 1.70 (IMP XI) and in between 0.8-1.3 for all other impurities. The LOD of the developed method for all the analytes were in the range of 0.05 to 0.11 μg/mL and the LOQ values were in the range of 0.17 to 0.36 μg/mL.

scholarly journals STABILITY INDICATING RP-LC ASSAY METHOD FOR CARISOPRODOL

2017 ◽  
Vol 9 (6) ◽  
pp. 79
Author(s):  
M. Sangeetha ◽  
Tirumala . ◽  
Nagamallika .
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Hplc Method ◽  
Assay Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Ich Guidelines ◽  
The Mean

Objective: A reverse phase stability-indicating HPLC method was developed for the determination of Carisoprodol in pharmaceutical dosage forms. The chromatographic elution was achieved on C18, 250 mm × 4.6 mm, 5-μm particle size column.Methods: The mobile phase contains a mixture of water and acetonitrile in ratio of 60:40 v/v. The flow rate was 1.0 ml min-1 and was detected by Refractive index detector.Results: The method was proven to be linear over a range of 1 to 4 mg/ml with a mean correlation coefficient of 0.99998. The %mean recovery is in the range of 100.55% to 101.11% and %RSD was less than 1.0% between preparations. The % RSD for Assay results of initial sample preparation in different intervals of 0hr, 24 h, 30 h and 48 h was less than 1.0%. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from Carisoprodol.Conclusion: The developed method was validated as per international ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness.

scholarly journals Development and validation of the stability-indicating LC-UV method for the determination of cefoselis sulphate

2012 ◽  
Vol 10 (1) ◽  
pp. 121-126 ◽  
Author(s):  
Przemysław Zalewski ◽  
Judyta Cielecka-Piontek ◽  
Anna Jelińska
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Kinetic Studies ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation

AbstractThe stability-indicating LC assay method was developed and validated for quantitative determination of cefoselis sulphate in the presence of degradation products formed during the forced degradation studies. An isocratic, RP-HPLC method was developed with C-18 (250 × 4.6 mm, 5 µm) column and 12 mM ammonium acetate-acetonitrile (95:5 V/V) as a mobile phase. The flow rate of the mobile phase was 1.0 mL min−1. Detection wavelength was 260 nm and temperature was 30°C. Cefoselis similarly to other cephalosporins was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness. The method was applied successfully for identification and determination of cefoselis sulphate in pharmaceuticals and during kinetic studies.

scholarly journals STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF CLEVIDIPINE BUTYRATE IN SYNTHETIC MIXTURE

2018 ◽  
Vol 10 (6) ◽  
pp. 159
Author(s):  
Charu P. Pandya ◽  
Sadhana J. Rajput
Keyword(s):  
Degradation Products ◽  
Standard Addition ◽  
Retention Factor ◽  
Economic Stability ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate stability indicating HPTLC method for determination of clevidipine butyrate in synthetic mixture.Methods: The present study deals with development and validation of stability indicating HPTLC method for estimation of clevidipine butryate. Chromatographic separation was performed on aluminum plate pre coated with Silica Gel 60 F254 using toluene: ethyl acetate (8:2) as mobile phase. TLC scanner was set at wavelength of 370 nm.Results: Retention factor Rf of clevidipine was found to be 0.49. The method was validated as per ICH guidelines. Calibration curve was in the range of 1000-6000ng/band. The correlation coefficient was found to be 0.999. The precision expressed by RSD was less than 2%. The accuracy of method was confirmed by recovery studies using standard addition method and recovery was found to be 99.03-99.57%. The drug was subjected to ICH prescribed hydrolytic, oxidative, photolytic and thermal stress conditions. Clevidipine and its degradation products were well resolved under experimental conditions. The method was validated according to ICH guidelines. The drug showed significant degradation in alkaline and acidic condition and slight degradation in oxidative condition. The drug was stable in thermal condition.Conclusion: A new, Simple, Accurate, Precise, Sensitive and economic stability indicating HPTLC method has been developed and validated for the determination of clevidipine and can be employed for stability indicating analysis.

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.

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