Abstract

A method involving the gas chromatographic separation of the trimethylsilyl derivatives of possible intermediates in the biosynthesis of cyanogenic glucosides and the determination of the radioactivity in the individual compounds by use of a gas proportional counter is described. The trimethylsilyl derivatives were prepared by reacting lyophilized assay mixtures with bis-(trimethylsilyl)-trifluoroacetamide using acetonitrile as a reaction solvent. Gas chromatographic separation was accomplished with a 3% SP-2250 glass column and temperature programming. The organic material in the chromatographic effluent was oxidized to carbon dioxide and water by passing it through an oven containing cupric oxide, and the carbon dioxide was counted in a gas proportional counter. Structures of the trimethylsilyl derivatives were confirmed by combined gas chromatography—mass spectrometry.

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