Stability-Indicating RP-UPLC Method Development and Validation for the Process Related Impurities of Nebivolol and Structural Characterization of Its Forced Degradation Products by LC-MS/MS

2016 ◽  
Vol 14 (6) ◽  
pp. 1-13
Author(s):  
Prasad Kancherla ◽  
Pallavi Alegete ◽  
Srinivas Keesari ◽  
Bhavyasri Khagga ◽  
Sridhar Siddiraju ◽  
...  
Keyword(s):  
Structural Characterization ◽  
Method Development ◽  
Degradation Products ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Related Impurities ◽  
Method Development And Validation ◽  
Development And Validation

scholarly journals Identification and Characterization of Two New Forced Degradation Products of Saikosaponin a under the Stress of Acid Hydrolytic Condition

2016 ◽  
Author(s):  
Jun Li ◽  
Qiang Xu ◽  
Hua Jiang
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Forced Degradation ◽  
Worst Case ◽  
Method Performance ◽  
Stability Indicating Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Saikosaponin A

Saikosaponin (SS) a is a compound with various pharmacological properties and easily degraded into SSb1 and SSg in acid condition. In present work another two new degradation products of SSa formed under acid hydrolytic condition were detected and isolated by analytical and semi-preparative liquid chromatography technology, furthermore their structures were characterized as hydroxyl-saikosaponin a and SSb2 by spectral analysis, which is not only essential in stability-indicating method development and validation but also could be used as a worst case to assess the analytical method performance of SSa. Moreover their structural transformation pathways were also proposed.

scholarly journals Isolation, Identification and Characterization of Gefitinib Novel Degradation Products by NMR and HRMS, Method Development and Validation by UPLC

2021 ◽  
Vol 33 (8) ◽  
pp. 1743-1748
Author(s):  
Ramulu Yanaka ◽  
Hima Bindu Gandham ◽  
Chidananda Swamy Rumalla ◽  
Muralidharan Kaliyaperumal ◽  
Shaik John Saida ◽  
...  
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
2D Nmr ◽  
The Novel ◽  
Ich Guidelines ◽  
Stress Degradation ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Identification And Characterization

Gefitinib (GFT) sold under the brand name Iressa, is a medication used to treat certain type of breast, lung and other cancers, Gefitinib was subject to stress degradation under acidic, basic, peroxide mediated oxidation, photolytic and thermal degradation. The stress degradation was performed according to ICH guidelines Q1A(R2) and the drug was inert under thermal and photolytic conditions. One degradant is identified in acid hydrolysis referred as 7-methoxy-6-(3-morpholinopropoxy) quinazolin-4(3H)-one (GFT-DP1) and two degradants were formed in peroxide mediated hydrolysis referred as 4-(3-((4-((3- chloro-4-fluorophenyl)amino)-7-methoxy-1-oxidoquinazolin-6-yl)oxy)-propyl)morpholine-4-oxide (GFT-DP2) and 4-(3-((4-((3-chloro-4-fluorophenyl)amino)-7-methoxyquinazolin-6-yl)oxy)-propyl)- morpholine-4-oxide (GFT-DP3). In present study, all the novel three degradation product structures were confirmed by HRMS and 1D (1H, 13C) and 2D (COSY, HSQC and HMBC) based on 1D and 2D NMR data proton and carbon chemical shift values assigned exactly for all degradation products. A stability indicating RP-UPLC method was developed and validated with shorter run time and this method was validated in terms of linearity, specificity, accuracy, LOD and LOQ.

scholarly journals LC–MS/MS characterization of the forced degradation products of ezetemibe: Development and validation of a stability-indicating UPLC method

2016 ◽  
Vol 10 (1) ◽  
pp. 148-160 ◽  
Author(s):  
Prasad Kancherla ◽  
Venkatappaiah Velpuri ◽  
Pallavi Alegete ◽  
Saeed S. Albaseer ◽  
Mukkanti Khagga ◽  
...  
Keyword(s):  
Degradation Products ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Development And Validation
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