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 Stability indicating method development and validation for simultaneous estimation and quantification of Ertugliflozin and Metformin in bulk and tablet dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Bhawani Sunkara ◽  
Tulja Rani Gampa ◽  
Mounika Markanti ◽  
Ratna Kumari Midthapally
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Simultaneous Estimation ◽  
Elution Time ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Simultaneous Evaluation ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

Abstract Background A simple, economical, sensitive, authentic, and faithful technique was used for the study of simultaneous evaluation of Ertugliflozin and Metformin in tablet dosage forms. The Chromatographic analysis was performed isocratically by using a Phenomenex C18 column (150 mm × 4.6 mm, 5 μm), and a mobile phase containing acetonitrile and 0.1% OPA buffer, with a proportion of 40: 60% v/v was passed throughout the column maintained at a temperature of 30 °C with a flow rate of 1 ml/min. Approximately, 10 μl of drug solution was injected and the analytes were eluted at 220.0 nm. Results The elution times of Ertugliflozin and Metformin were 2.226 min and 2.955 min, respectively. The percentage RSD of Ertugliflozin and Metformin are 0.60 and 0.59, respectively. The percentage recoveries of Ertugliflozin and Metformin were determined to be 100.55% and 99.40%, respectively. LOD, LOQ values of Metformin and Ertugliflozin obtained were found to be 0.10, 0.2 μg/ml and 0.03, 0.09 μg/ml, respectively. Regression equation of Ertugliflozin was y = 11287x + 1191 and y = 46270x + 161.0 for Metformin. All verification parameters are within the range according to the ICH guidelines, and the degradation products are also within the limits, which show that the method is stable. Conclusion In the currently developed RP-HPLC analytical method, the elution time and run time is reduced, which proves that the method is economical and widely acceptable, also simple and practical, which can be used in routine quality control tests in the industry.

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