Degradation of ouabain in 80-year-old injection solution studied by HILIC–MS
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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.
KeywordsHigh-performance liquid chromatography Decomposition Long-term stability Mass spectrometry g-Strophanthin
The financial support by the projects SVV and Progress Q46 of Charles University is gratefully acknowledged.
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