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

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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.

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Acknowledgements

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

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Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Science, Charles University, Prague, Czech Republic

    Karel Kudláček, Karel Nesměrák & Petr Kozlík

  2. Department of Chemistry, Faculty of Science, Charles University, Prague, Czech Republic

    Martin Štícha

  3. Czech Pharmaceutical Museum, Faculty of Pharmacy in Hradec Králové, Charles University, Kuks, Czech Republic

    Jan Babica

Authors
  1. Karel Kudláček
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  2. Karel Nesměrák
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  3. Martin Štícha
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  4. Petr Kozlík
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  5. Jan Babica
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Corresponding author

Correspondence to Karel Nesměrák.

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Kudláček, K., Nesměrák, K., Štícha, M. et al. Degradation of ouabain in 80-year-old injection solution studied by HILIC–MS. Monatsh Chem 149, 1555–1560 (2018). https://doi.org/10.1007/s00706-018-2216-9

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  • DOI: https://doi.org/10.1007/s00706-018-2216-9

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