Characterization of the degradation products of bambuterol using LCMS-QTOF and NMR

A systematic forced degradation study of bambuterol was carried out according to ICH guidelines. Twelve degradation products of bambuterol were identified and characterized. Plausible mechanisms of formation of the degradation products are discussed.

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Synthesis and Characterization of Potential and Degraded Impurities of Regadenoson

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190819095255 ◽

2020 ◽

Vol 16 (8) ◽

pp. 1130-1139

Author(s):

Singaram Sathiyanarayanan ◽

Chidambaram Subramanian Venkatesan ◽

Senthamaraikannan Kabilan

Keyword(s):

Mass Spectra ◽

Degradation Products ◽

Hplc Method ◽

Forced Degradation ◽

Spectroscopic Techniques ◽

A2a Adenosine Receptor ◽

Degradation Study ◽

Related Substances ◽

Adenosine Receptor Agonist

Background: Regadenoson is an A2A adenosine receptor agonist that is a coronary vasodilator and commonly used as a pharmacologic cardiac stressing agents. Methods: HPLC method was used for the analysis of related substances. The degraded impurities during the process were isolated and characterized by IR, Mass and NMR spectral analysis. Results: Forced degradation study of regadenoson under conditions of hydrolysis (neutral, acidic and alkaline) and oxidations suggested in the ICH Q1A(R2) was accomplished. The drug showed significant degradation under all the above conditions. On the whole, five novel degradation products were found under diverse conditions along with process related impurities which were not reported earlier. Conclusion: All the degradation products were well characterized by using advanced spectroscopic techniques like IR, 1H NMR, 13C NMR and Mass spectra. The identification of these impurities will be productive for the quality control during the production and stability behavior of the regadenoson drug substance.

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Identification and structural characterization of the stress degradation products of omeprazole using Q-TOF-LC-ESI-MS/MS and NMR experiments: evaluation of the toxicity of the degradation products

New Journal of Chemistry ◽

10.1039/c9nj00932a ◽

2019 ◽

Vol 43 (19) ◽

pp. 7294-7306 ◽

Cited By ~ 2

Author(s):

G. Shankar ◽

Roshan M. Borkar ◽

Suresh Udutha ◽

M. Kanakaraju ◽

G. Sai Charan ◽

...

Keyword(s):

Gastroesophageal Reflux Disease ◽

Proton Pump Inhibitor ◽

Gastroesophageal Reflux ◽

Degradation Products ◽

Forced Degradation ◽

Peptic Ulcers ◽

Ich Guidelines ◽

Stress Degradation ◽

Forced Degradation Studies

Omeprazole (OMP), a prototype proton pump inhibitor used for the treatment of peptic ulcers and gastroesophageal reflux disease (GERD), was subjected to forced degradation studies as per ICH guidelines Q1A (R2).

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Characterization of stress degradation products of blonanserin by UPLC-QTOF-tandem mass spectrometry

RSC Advances ◽

10.1039/c5ra10641a ◽

2015 ◽

Vol 5 (85) ◽

pp. 69273-69288 ◽

Cited By ~ 3

Author(s):

Pradipbhai D. Kalariya ◽

Prinesh N. Patel ◽

Mahesh Sharma ◽

Prabha Garg ◽

R. Srinivas ◽

...

Keyword(s):

Mass Spectrometry ◽

High Resolution ◽

Tandem Mass Spectrometry ◽

Degradation Products ◽

Structural Elucidation ◽

Forced Degradation ◽

Tandem Mass ◽

Degradation Study ◽

Stress Degradation

Forced degradation study of blonanserin and structural elucidation of its degradation products was performed using high resolution tandem mass spectrometry.

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LC-MS/MS CHARACTERIZATION OF FORCED DEGRADATION PRODUCTS OF TUCATINIB, A NOVEL TYROSINE KINASE INHIBITOR: DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2022v14i1.43252 ◽

2022 ◽

pp. 58-66

Author(s):

S. K. REEHANA ◽

K. SUJANA

Keyword(s):

Kinase Inhibitor ◽

Degradation Products ◽

Degradation Pathway ◽

Hplc Method ◽

Forced Degradation ◽

Ich Guidelines ◽

System Suitability ◽

Forced Degradation Studies ◽

Development And Validation

Objective: The current study focused on the development, validation, and characterization of forced degradation products using LC-MS/MS. Methods: A simple, selective, validated and well-defined isocratic HPLC methodology for the quantitative determination of Tucatinib at a wavelength of 239 nm. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6 mm, 5m) column with a mobile phase of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 ml/min. MS/MS was used to characterize degradation products formed in the forced degradation study. The validation and characterization of forced degradation products were performed in accordance with ICH guidelines. Results: Over the concentration range of 5-100μg/ml, a good linear response was obtained. Tucatinib's LOD and LOQ were determined to be 0.05 and 0.5, respectively. According to standard guidelines, the method was quantitatively evaluated in terms of system suitability, linearity, precision, accuracy, and robustness, and the results were found to be within acceptable limits. The drug was degraded under acidic, alkaline, and reduction conditions in forced degradation studies. Conclusion: The method was found to be applicable for routine tucatinib analysis. Because no LC-MS/MS method for estimating tucatinib and its degradation products has been reported in the literature. There is a need to develop a method for studying the entire tucatinib degradation pathway.

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