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.
- 2.Carstensen JT, Rhodes C (2000) Drug stability. Principles and practices, 3rd edn. Marcel Dekker, New YorkGoogle Scholar
- 3.Yoshioka S, Stella VJ (2002) Stability of drugs and dosage forms. Kluwer, New YorkGoogle Scholar
- 8.Jordi Gonzalez R (1989) Farm Clin 6:451Google Scholar
- 20.Haskell CC, Doeppers WA (1914) J Am Pharm Assoc 3:646Google Scholar
- 21.Pomeroy CA, Heyl FW (1922) Am J Pharm 94:479Google Scholar
- 24.Berry H (1935) Q J Pharm Pharmacol 8:464Google Scholar
- 25.Tajiri Y, Dosako K, Matsumoto Y, Goya K, Kurata M, Shinohara C (1978) Hiroshima-ken Byoin Yakuzaishikai Gakujutsu Nenpo 13:54Google Scholar