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LC-ESI-MS/MS characterization of strophanthin-K
Giorgio Grosa1, Gianna Allegrone, Erika Del Grosso
1Dipartimento di Scienze Chimiche, Alimentari, Farmaceutiche e Farmacologiche-Università degli Studi del Piemonte Orientale "Amedeo Avogadro", Via Bovio 6, 28100 Novara, Italy.
Journal of Pharmaceutical and Biomedical Analysis
|May 24, 2005
Summary
A new liquid chromatography-mass spectrometry (LC-MS) method characterizes strophanthin-K cardiac glycosides from Strophanthus kombe seeds. It identifies six glycosides and reveals degradation pathways under acidic and basic conditions.
Area of Science:
- Pharmacognosy
- Analytical Chemistry
- Natural Products Chemistry
Background:
- Strophanthin-K, a mixture of cardiac glycosides from Strophanthus kombe seeds, possesses significant medicinal properties.
- Accurate characterization of these complex glycosides is crucial for quality control and pharmacological studies.
- Existing analytical methods may lack the sensitivity or specificity required for comprehensive strophanthin-K analysis.
Purpose of the Study:
- To develop and validate a robust liquid chromatography-mass spectrometry (LC-MS) method for the characterization of strophanthin-K.
- To identify and quantify major cardiac glycosides within the strophanthin-K extract.
- To investigate the degradation pathways of strophanthin-K under various conditions.
Main Methods:
- High-performance liquid chromatography (HPLC) coupled with electrospray ionization mass spectrometry (ESI-MS) was employed.
- A RP C-18 column was used with a gradient mobile phase of water, 1% formic acid in water, and acetonitrile.
- Analysis was performed in negative ion mode, utilizing adduct ion formation ([M+HCOO](-)) and MS/MS for pseudomolecular ions ([M-H](-)).
Main Results:
- The LC-MS method successfully separated and characterized six cardiac glycosides: k-strophanthoside, k-strophanthin-beta, helveticoside (erysimin), erysimoside, cymarin, and neoglucoerysimoside.
- ESI-MS in negative ion mode yielded abundant [M+HCOO](-) adducts, while ESI-MS/MS provided [M-H](-) pseudomolecular ions.
- Forced degradation studies indicated k-strophanthidin as the primary aglycone product under acidic conditions, and lactone hydrolysis to gamma-hydroxy acids under basic conditions.
Conclusions:
- The developed LC-MS method provides a sensitive and specific approach for the characterization of strophanthin-K and its constituent cardiac glycosides.
- The study identified key glycosides and elucidated their degradation behavior, essential for understanding their stability and potential therapeutic applications.
- This analytical framework supports the quality assessment and further research into the pharmacological potential of Strophanthus kombe-derived compounds.