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Development and validation of a stability-indicating HPLC assay method for determination of ethacrynic acid in solution formulation. HPLC-MS identification of hydrolytic and oxidative degradation products

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Degradation products of ethacrynic acid
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Submitted   Jul 19, 2020
Published   Aug 31, 2020
Issue    Vol 2 No 1 (2020)
DOI   10.25082/JPBR.2020.01.005

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Mónika Kuzma corresponding author
Institute of Pharmaceutical Chemistry, University of Pécs, Rókus Str. 2, Pécs 7624, Hungary & Department of Forensic Medicine, University of Pécs, Medical School, Szigeti Str. 12, Pécs 7624, Hungary
Veronika Murányi
Institute of Pharmaceutical Chemistry, University of Pécs, Rókus Str. 2, Pécs 7624, Hungary
Mátyás Mayer
Department of Forensic Medicine, University of Pécs, Medical School, Szigeti Str. 12, Pécs 7624, Hungary
Zsuzsanna Rozmer
Institute of Pharmaceutical Chemistry, University of Pécs, Rókus Str. 2, Pécs 7624, Hungary
Pál Perjési
Institute of Pharmaceutical Chemistry, University of Pécs, Rókus Str. 2, Pécs 7624, Hungary

Abstract

An isocratic stability-indicating HPLC assay method was developed to quantitate ethacrynic acid in solution formulations. Utilizing the method, the main hydrolytic, and one of the oxidative degradation products could be separated. The structure of the separated degradation products was confirmed by negative ion-mode HPLC-MS. The hydrolytic results confirmed the previously reported sequence of the formation of the dimeric Michael adduct. One new oxidative metabolite has been identified. The validated analytical method can be used to quantitate ethacrynic acid in a solution formulation in the 0.5-500 µg/ml concentration range.

Keywords
forced degradation, hydrolytic degradation products, oxidative degradation products, michael addition reaction, stability-indicating HPLC method, HPLC-MS

Article Details

Supporting Agencies
This work was supported by the National Office of Research and Technology, “Pázmány Péter program” (RET-II 08/2005), the European Union, co-financed by the European Social Fund (EFOP-3.6.1.-16-2016-00004).
How to Cite
Kuzma, M., Murányi, V., Mayer, M., Rozmer, Z., & Perjési, P. (2020). Development and validation of a stability-indicating HPLC assay method for determination of ethacrynic acid in solution formulation. HPLC-MS identification of hydrolytic and oxidative degradation products. Journal of Pharmaceutical and Biopharmaceutical Research, 2(1), 131-144. https://doi.org/10.25082/JPBR.2020.01.005
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This work is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.

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