Summary
Analysis of minor compounds in spirits is a difficult problem. Whereas isopentanols are present at the g/l level, carbonyl compounds are, with the exception of ethanal, at the ppb level.
In this work the first step is the use of pentafluorobenzyl hydroxylamine as a reagent which leads to 0-pentafluorobenzyl oximes with Cognac carbonyl compounds. The second step is the selective reduction of the C=N double bond with a pyridine/borane complex, generating 0-pentafluorobenzylamines and a single peak on GC chromatograms. The SIM detection at m/z 181 by GC-MS at 35 eV allows quantitative determination at the ppb level with a 200 ml sample.
The reproductibility of the method is 20% at the 10 ppb level. The method is useful for the quantitative analysis of aldehydes and ketones. An example of the determination of methyl ketones in aged Cognac is given, together with quantitative data.
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Vidal, J.P., Estreguil, S. & Cantagrel, R. Quantitative analysis of Cognac carbonyl compounds at the PPB level by GC-MS of their 0-(pentafluorobenzyl amine) derivatives. Chromatographia 36, 183–186 (1993). https://doi.org/10.1007/BF02263859
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DOI: https://doi.org/10.1007/BF02263859