Gas Chromatographic and Mass Spectrometric Study of Trimethylsilyl Ethers of Cardiac Aglycones

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Abstract
Cardenolides may be converted to volatile derivatives by silylation. Three levels of silylation have been defined. The use of HMDS-TMCS leads to TMSi ether formation for all relatively unhindered hydroxyl groups (3β, 12β, 16β). When BSA-TMCS is employed, the unsaturated lactone ring is converted to an enol form, with subsequent formation of a TMSi enol ether. All hydroxyl groups, including the tert. 14β-hydroxyl group and the enol derived from the lactone side chain, are converted to TMSi ethers with TSIM-BSA-TMCS at 60°. The derivatives have good gas chromatographic properties. Gas phase analytical methods can be used for the identification and characterization of these substances.