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.

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 QUANTIFICATION OF THE COMPONENTS IN COMMERCIAL ESSENTIAL OIL OF EUCALYPTUS GLOBULUS LABILL. BY GAS CHROMATOGRAPHY – GC-FID AND GC-MS

2017 ◽  
Vol 1 (2) ◽  
pp. 9-14
Author(s):  
Miriam Anders Apel ◽  
Rodney A.F. Rodrigues ◽  
Luiz Alberto Lira Soares ◽  
Amélia Terezinha Henriques
Keyword(s):  
Gas Chromatography ◽  
Essential Oil ◽  
High Sensitivity ◽  
Symptomatic Treatment ◽  
Fused Silica ◽  
Flame Ionization ◽  
Fused Silica Capillary ◽  
Main Component ◽  
Chemical Quantification ◽  
Silica Capillary

Leaves of Eucalytus globulus Labill are characterized by the presence of essential oil, in which 1,8-cineole is the main component. The oil is used as an expectorant for symptomatic treatment of mild inflammation of the respiratory tract and bronchitis. This work addresses the chemical quantification of the constituents of E. globulus essential oil by gas chromatography. Commercial samples were diluted and analyzes by gas chromatograph coupled to flame ionization detector (GC-FID). The chromatographic separation was performed on a fused silica capillary (LM-20, 30 m x 0.25 mm x 0.25 μm film thickness) column. The proposed GC-FID method has demonstrated to have specificity and high sensitivity. The quantitation by the normalization technique demonstrated to be adequate for the analysis. Thus, the proposed method is effective for the quantification of E. globulus oil constituents, which may help in the quality control of commercial formulations.

Stability-Indicating Method Development and Validation for Busulfan Drug Substance by Gas Chromatography-Flame Ionization Detector

2020 ◽  
Author(s):  
Ashraf Khan ◽  
Greg Winter ◽  
Shane Tan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Fused Silica ◽  
Drug Substance ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Flame Ionization ◽  
Stability Indicating Method ◽  
Organic Impurities ◽  
Chromatographic Parameters

Abstract A new, simple and stability-indicating gas chromatography-flame ionization detection (GC-FID) method was developed and validated for the quantitative determination of busulfan and its organic impurities (OI) in drug substance without derivatization. The chromatographic attributes were achieved on a fused silica capillary column (0.53 mm × 30 m, 1.0 μm, USP Phase G42), using hydrogen as a carrier gas with a split ratio of 1:1. Forced degradation studies were conducted to establish the stability-indicating capability and method specificity that showed the stressed busulfan peak was free from any co-elution. Robustness study demonstrated the chromatograms remained mostly unaffected under deliberate, but small variations of chromatographic parameters, establishing the reliability of the method during routine usage. The method was shown to be reliable, sensitive, specific, linear, accurate, precise and rugged in the 1,4-butanediol concentration range of 1–20 μg/mL. The method, intended for compendial uses, is suitable for quantitative analysis of busulfan and its organic impurities in drug substances.

Stability-Indicating Micellar Electrokinetic Chromatography Technique for Simultaneous Measurement of Delapril and Manidipine from a Combination Drug Formulation

2014 ◽  
Vol 97 (1) ◽  
pp. 114-120 ◽  
Author(s):  
Vítor Todeschini ◽  
Maximiliano da Silva Sangoi ◽  
Alianise da Silva Meira ◽  
Diogo Miron ◽  
Alini Dall Cortivo Lange ◽  
...  
Keyword(s):  
Background Electrolyte ◽  
Sodium Dodecylsulfate ◽  
Internal Standard ◽  
Fused Silica ◽  
Drug Formulation ◽  
Effective Length ◽  
Forced Degradation ◽  
Combination Drug ◽  
Stability Indicating ◽  
Fused Silica Capillary

Abstract A stability-indicating micellar electrokineticchromatography (MEKC) method was developed and validated for simultaneous analysis of delapril (DEL) and manidipine (MAN) using salicylic acid as an internal standard. The MEKC method was performed using a fused-silica capillary (effective length of 72 cm) with 50 mM of borate buffer and 5 mM of anionic surfactant sodium dodecylsulfate at pH9.0 as the background electrolyte. The separationwas achieved at 25 kV applied voltage and 35°C. The injection was performed at 50 mbar for5s, with detection at 208 nm. The method was linear in the range of 15–150 μg/mL (r2 = 0.9966) for DEL and 5–50 μg/mL (r2 = 0.9985) for MAN with adequate results for the precision (≤1.87%) and accuracy (98.94% for DEL and 100.65% for MAN). The specificity of the method and its stability-indicating capability was demonstrated through forced degradation studies, which showed that there was no interference from the excipients. The Plackett-Burman experimental design was used for robustness evaluation, giving results within the acceptable range. The method was successfully applied for analysis of the drugs, and the results were compared to an LC method, resulting in nonsignificant differences (P = 0.78 and0.84 for DEL and MAN, respectively).

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