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

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.

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LC-MS/MS characterization of forced degradation products of ambrisentan: development and validation of a stability-indicating RP-HPLC method

New Journal of Chemistry ◽

10.1039/c4nj00075g ◽

2014 ◽

Vol 38 (7) ◽

pp. 3050 ◽

Cited By ~ 14

Author(s):

Nageswara Rao Ramisetti ◽

Ramakrishna Kuntamukkala

Keyword(s):

Degradation Products ◽

Hplc Method ◽

Forced Degradation ◽

Stability Indicating ◽

Rp Hplc ◽

Development And Validation

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

Asian Journal of Chemistry ◽

10.14233/ajchem.2021.23210 ◽

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.

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