Stress degradation of edaravone: Separation, isolation and characterization of major degradation products

Stress degradation of edaravone: Separation, isolation and characterization of major degradation... In the present study the International Conference on Harmonization‐prescribed stress degradation was carried out to study the degradation profile of edaravone. To establish a Quality by Design (QbD)‐assisted stability‐indicating assay, the reaction solutions in which different degradation products were formed were mixed. Plackett Burman and central composite design were used to screen and optimize experimental variables to resolve edaravone and its impurities with good peak symmetry using an RP C18 column. The method was validated according to International Conference on Harmonization guidelines. Seven unknown and two known degradation products were identified and characterized by LC‐MS/MS. Two major degradation products formed under thermal degradation were isolated and characterized as 4‐(4,5‐dihydro‐3‐methyl‐5‐oxo‐1‐phenyl‐1H‐pyrazol‐4‐yl‐4‐(4,5‐dihydro‐5‐hydroxy‐3‐methyl‐1‐phenyl‐1H‐pyrazol‐4‐yl)‐3‐methyl‐1‐phenyl‐1H‐pyrazol‐5(4H)‐one and 3‐hydroxy‐dihydro‐thiazolo[1‐(2‐methyl‐buta‐1,3dienyl)‐1‐phenylhydrazine]5‐one. The degradation pathways of degradants were proposed based on m/z values. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Biomedical Chromatography Wiley

Stress degradation of edaravone: Separation, isolation and characterization of major degradation products

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Publisher
Wiley Subscription Services, Inc., A Wiley Company
Copyright
Copyright © 2018 John Wiley & Sons, Ltd.
ISSN
0269-3879
eISSN
1099-0801
D.O.I.
10.1002/bmc.4146
Publisher site
See Article on Publisher Site

Abstract

In the present study the International Conference on Harmonization‐prescribed stress degradation was carried out to study the degradation profile of edaravone. To establish a Quality by Design (QbD)‐assisted stability‐indicating assay, the reaction solutions in which different degradation products were formed were mixed. Plackett Burman and central composite design were used to screen and optimize experimental variables to resolve edaravone and its impurities with good peak symmetry using an RP C18 column. The method was validated according to International Conference on Harmonization guidelines. Seven unknown and two known degradation products were identified and characterized by LC‐MS/MS. Two major degradation products formed under thermal degradation were isolated and characterized as 4‐(4,5‐dihydro‐3‐methyl‐5‐oxo‐1‐phenyl‐1H‐pyrazol‐4‐yl‐4‐(4,5‐dihydro‐5‐hydroxy‐3‐methyl‐1‐phenyl‐1H‐pyrazol‐4‐yl)‐3‐methyl‐1‐phenyl‐1H‐pyrazol‐5(4H)‐one and 3‐hydroxy‐dihydro‐thiazolo[1‐(2‐methyl‐buta‐1,3dienyl)‐1‐phenylhydrazine]5‐one. The degradation pathways of degradants were proposed based on m/z values.

Journal

Biomedical ChromatographyWiley

Published: Jan 1, 2018

Keywords: ; ; ; ;

References

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