Stability indicating spectrophotometric methods for determination of Tiemonium methylsulphate in the presence of its degradation products

2014 ◽  
Vol 4 (1) ◽  
pp. 33-45 ◽  
Keyword(s):  
Degradation Products ◽  
Stability Indicating ◽  
Spectrophotometric Methods

scholarly journals Development and validation of stability indicating method for determination of sodium citrate in pediatric cough syrup

2020 ◽  
Vol 8 (2) ◽  
pp. 213-223
Author(s):  
Abdrhman Mahmoud Gamil ◽  
Mohamed Awad al-lkareem Hamad
Keyword(s):  
Sodium Citrate ◽  
Degradation Products ◽  
Base Hydrolysis ◽  
Column Temperature ◽  
Stability Indicating ◽  
Spectrophotometric Methods ◽  
End Point ◽  
Regulatory Affairs ◽  
Stability Indicating Method

Sodium Citrate is widely used in analytical and food processes. It is used in various medical applications as anticoagulant in blood transfusion process and bladder washout. It is used in cough preparation as mucolytic. There are many methods for determination of Sodium Citrate in different preparations. Some of which use spectrophotometric methods, others used HPLC methods. The USP method uses titration and determining the end point potentionometrically. Many arguments take place between the Drug Regulatory Affairs and manufacturers regarding the appearance of the colour at the end point. The objective of this study is to develop and validate a simple, easy and precise HPLC stability indicating method for routine work and to be submitted to the Drug Regulatory Affairs. Chromatographic system with detector PDA at 210nm is utilized, Reprosil-XR C18, 250 mm×4 mm, 5 µm column is used. Column temperature 300C and flow rate of 1 ml/min. A clear peak of acceptable purity at 3.38 min retention time appears. The method is subjected to thermal stress, acid and base hydrolysis at extreme pH and forced oxidation. The result is that there is no interference of degradation products with the substance peak. The method is then subjected to validation study according to the ICH guidelines. The method comply the specificity, precision, linearity, accuracy and robustness acceptable criteria. Thus, the method satisfies the stability indicating method and validation requirements that it can be submitted to the Drug Regulatory Affairs and used in QC routine activities and stability studies.

scholarly journals Development and validation of stability indicating method for determination of sodium citrate in pediatric cough syrup

2020 ◽  
Vol 8 (2) ◽  
pp. 213-223
Author(s):  
Abdrhman Mahmoud Gamil ◽  
Mohamed Awad al-lkareem Hamad
Keyword(s):  
Sodium Citrate ◽  
Degradation Products ◽  
Base Hydrolysis ◽  
Column Temperature ◽  
Stability Indicating ◽  
Spectrophotometric Methods ◽  
End Point ◽  
Regulatory Affairs ◽  
Stability Indicating Method

Sodium Citrate is widely used in analytical and food processes. It is used in various medical applications as anticoagulant in blood transfusion process and bladder washout. It is used in cough preparation as mucolytic. There are many methods for determination of Sodium Citrate in different preparations. Some of which use spectrophotometric methods, others used HPLC methods. The USP method uses titration and determining the end point potentionometrically. Many arguments take place between the Drug Regulatory Affairs and manufacturers regarding the appearance of the colour at the end point. The objective of this study is to develop and validate a simple, easy and precise HPLC stability indicating method for routine work and to be submitted to the Drug Regulatory Affairs. Chromatographic system with detector PDA at 210nm is utilized, Reprosil-XR C18, 250 mm×4 mm, 5 µm column is used. Column temperature 300C and flow rate of 1 ml/min. A clear peak of acceptable purity at 3.38 min retention time appears. The method is subjected to thermal stress, acid and base hydrolysis at extreme pH and forced oxidation. The result is that there is no interference of degradation products with the substance peak. The method is then subjected to validation study according to the ICH guidelines. The method comply the specificity, precision, linearity, accuracy and robustness acceptable criteria. Thus, the method satisfies the stability indicating method and validation requirements that it can be submitted to the Drug Regulatory Affairs and used in QC routine activities and stability studies.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

scholarly journals Validated stability indicating methods for determination of nitazoxanide in presence of its degradation products

2012 ◽  
Vol 2 (2) ◽  
pp. 105-116 ◽  
Author(s):  
Nouruddin W. Ali ◽  
Samah Sayed Abbas ◽  
Hala El-Sayed Zaazaa ◽  
Maha Mohamed Abdelrahman ◽  
Mohamed Abdelkawy
Keyword(s):  
Degradation Products ◽  
Stability Indicating

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

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