Study of forced degradation behaviour of cobicistat and atazanavir using LC/ESI/QTOF/MS; a combination of in-sourced and collision-induced dissociation for evaluation of the fragmentation patterns of degradation products

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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LC-MS/MS method for the characterization of the forced degradation products of Entecavir

Journal of Separation Science ◽

10.1002/jssc.201300959 ◽

2014 ◽

Vol 37 (4) ◽

pp. 368-375 ◽

Cited By ~ 9

Author(s):

Thippani Ramesh ◽

Pothuraju Nageswara Rao ◽

Ramisetti Nageswara Rao

Keyword(s):

Degradation Products ◽

Forced Degradation

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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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Separation and Characterization of New Forced Degradation Products of Macitentan: A Dual Endothelin Receptor Antagonist

Chromatographia ◽

10.1007/s10337-018-3471-y ◽

2018 ◽

Vol 81 (3) ◽

pp. 525-531 ◽

Cited By ~ 2

Author(s):

Mohit Thummar ◽

Debasish Swain ◽

S. Gananadhamu

Keyword(s):

Receptor Antagonist ◽

Degradation Products ◽

Endothelin Receptor Antagonist ◽

Forced Degradation ◽

Endothelin Receptor

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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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