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 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 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.

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 Development and Validation of Stability-Indicating HPLC Methods for the Estimation of Lomefloxacin and Balofloxacin Oxidation Process under ACVA, H2O2, or KMnO4 Treatment. Kinetic Evaluation and Identification of Degradation Products by Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5251
Author(s):  
Barbara Żuromska-Witek ◽  
Paweł Żmudzki ◽  
Marek Szlósarczyk ◽  
Anna Maślanka ◽  
Urszula Hubicka
Keyword(s):  
Room Temperature ◽  
Oxidation Process ◽  
Degradation Products ◽  
Isocratic Elution ◽  
Kinetic Evaluation ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Azo Initiator ◽  
Development And Validation ◽  
Kinetics Of

The oxidation of lomefloxacin (LOM) and balofloxacin (BAL) under the influence of azo initiator of radical reactions of 4,4′-azobis(4-cyanopentanoic acid) (ACVA) and H2O2 was examined. Oxidation using H2O2 was performed at room temperature while using ACVA at temperatures: 40, 50, 60 °C. Additionally, the oxidation process of BAL under the influence of KMnO4 in an acidic medium was investigated. New stability-indicating HPLC methods were developed in order to evaluate the oxidation process. Chromatographic analysis was carried out using the Kinetex 5u XB—C18 100A column, Phenomenex (Torrance, CA, USA) (250 × 4.6 mm, 5 μm particle size, core shell type). The chromatographic separation was achieved while using isocratic elution and a mobile phase with the composition of 0.05 M phosphate buffer (pH = 3.20 adjusted with o-phosphoric acid) and acetonitrile (87:13 v/v for LOM; 80:20 v/v for BAL). The column was maintained at 30 °C. The methods were validated according to the ICH guidelines, and it was found that they met the acceptance criteria. An oxidation process followed kinetics of the second order reaction. The most probable structures of LOM and BAL degradation products formed were assigned by the UHPLC/MS/MS method.

scholarly journals Ultra performance liquid chromatographic method for simultaneous quantitation of degradation products of telmisartan and hydrochlorothiazide in combination dosage form

2020 ◽  
Vol 11 (2) ◽  
pp. 2070-2082
Author(s):  
Narasimha Reddy G P ◽  
Sreenivasulu Reddy T ◽  
Sidda Reddy K ◽  
Shashi Kumar K N
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Wave Length ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

This work is intended to thrive a stability indicating Ultra performance liquid method for the estimation of (TLM) and (HCTZ) and degradation products pharmaceutical dosage forms. Separation was carried out on Zorbax Eclipse XDB C-18(50 x 2.1 mm, 1.7 ) column using a gradient method. Mobile phase A is 10mM KH2PO4 having 1% (v/v) of and mobile phase B is used in this work. 0.5 / minute is the flow of rate and at 271nm noticed wave length is monitored. Method development trails were carried out on six different columns. For specificity, limit of quantification, limit of detection, linearity, accuracy, method precision, robustness and stability this method is validated. Correlation coefficient of the impurities is more than 0.99. Stability indicating method confirmed that there were no interference of all impurities of TLM and HCTZ. Hence, developed LC method was stability indicating and well applied for drug product stability study as well as to quality monitoring.

Development and Validation of Stability-indicating Reverse Phase HPLC Assay for Tramadol in Bulk and Tablet Formulations

2019 ◽  
Vol 12 (3) ◽  
pp. 4544-4552
Author(s):  
Pankaj Padmakar Nerkar ◽  
Vaishali Badjuar ◽  
Pradyum Ige ◽  
Hitendra Mahajan ◽  
Sameer Ansari
Keyword(s):  
Orthophosphoric Acid ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Tablet Formulations ◽  
Development And Validation

This manuscript describes the development and validation of a simple, isocratic, and accurate reversed-phase HPLC method for the assay of tramadol in bulk powder form and tablet formulations. The chromato-graphic separation was achieved on an Qualisil BDS C18 (250 mm x 4.6mm, 5μm) column using acetonitrile: methanol: phosphate buffer pH 3.4 adjusted with orthophosphoric acid: (20:10:70, v/v) as a mobile phase, at a flow rate of 1 mL/min and detection at 271 nm. The linear range for tramadol were 2.0 to 10 μg/mL was obtained with correlation coefficients ≥ 0.999. The retention time was found to be 4.47 min for tramadol that was subjected to stress conditions, such as hydrolysis, oxidation, photolysis and thermal degradation, and the stressed samples were analyzed using the above methodology. The method was validated for the precision, accuracy, linearity and robustness. The developed stability-indicating method for tramadol was validated as per ICH guidelines.

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.

Development and Validation of a Stability Indicating RP-HPLC Method for Hydrocortisone Acetate Active Ingredient, Propyl Parahydroxybenzoate and Methyl Parahydroxybenzoate Preservatives, Butylhydroxyanisole Antioxidant, and Their Degradation Products in a Rectal Gel Formulation

2015 ◽  
Vol 98 (1) ◽  
pp. 27-34 ◽  
Author(s):  
Magda Ascaso ◽  
Pilar Pérez-Lozano ◽  
Mireia García ◽  
Encarna García-Montoya ◽  
Montse Miñarro ◽  
...  
Keyword(s):  
Active Ingredient ◽  
Active Substance ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Hydrocortisone Acetate ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability

Abstract A stability indicating method was established through a stress study, wherein different methods of degradation (oxidation, hydrolysis, photolysis, and temperature) were studied simultaneously to determine the active ingredient hydrocortisone acetate, preservatives propyl parahydroxybenzoate, and methyl parahydroxybenzoate, antioxidant butylhydroxyanisole (BHA), and their degradation products in a semisolid dosage gel form. The proposed method was suitably validated using a Zorbax SB-Phenyl column and gradient elution. The mobile phase consisted of a mixture of methanol, acetonitrile, and water in different proportions according to a planned program at a flow rate of 1.5 mL/min. The diode array detector was set at 240 nm for the active substance and two preservatives,and 290 nm for BHA. The validation study was conducted according to International Conference on Harmonization guidelines for specificity, linearity, repeatability, precision, and accuracy. The method was usedfor QC of hydrocortisone acetate gel and for the stability studies with the aim of quantifying the active substance, preservatives, antioxidant, and degradation products. It has proved to be suitable as a fast and reliable method for QC.

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