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Monatshefte für Chemie - Chemical Monthly

, Volume 149, Issue 9, pp 1555–1560 | Cite as

Degradation of ouabain in 80-year-old injection solution studied by HILIC–MS

  • Karel Kudláček
  • Karel Nesměrák
  • Martin Štícha
  • Petr Kozlík
  • Jan Babica
Original Paper
  • 59 Downloads

Abstract

An 80-year-old injection solution of ouabain was analyzed using HPLC–MS. A new separation method involving hydrophilic interaction liquid chromatography (HILIC) using an amide-based stationary phase with mass spectrometric detection was developed for the analysis. The optimized mobile phase composition was acetonitrile:water 85:15 (v/v) at the flow rate of 0.2 cm3/min under the isocratic elution. The ouabain content was found reduced to 56% of declared content and probable degradation product with oxidized hydroxy group was established. The ESI-MS2 fragmentation mechanism of ouabain was proposed.

Graphical abstract

Keywords

High-performance liquid chromatography Decomposition Long-term stability Mass spectrometry g-Strophanthin 

Notes

Acknowledgements

The financial support by the projects SVV and Progress Q46 of Charles University is gratefully acknowledged.

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Copyright information

© Springer-Verlag GmbH Austria, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Department of Analytical Chemistry, Faculty of ScienceCharles UniversityPragueCzech Republic
  2. 2.Department of Chemistry, Faculty of ScienceCharles UniversityPragueCzech Republic
  3. 3.Czech Pharmaceutical Museum, Faculty of Pharmacy in Hradec KrálovéCharles UniversityKuksCzech Republic

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