35-5/Clark/Derivatization Solid-Phase Microextraction...

Published: Journal of Chromatographic Science, Volume 35, Number 5, May 1997, pp. 209–212.

Derivatization Solid-Phase Microextraction Gas Chromatographic–Mass Spectrometric Determination of Organic Acids in Tobacco
T.J. Clark and J.E. Bunch

Isovaleric, valeric, hexanoic, benzoic, phenylacetic, 3-methylvaleric, heptanoic, octanoic, and nonanoic acids are converted to their methyl esters and quantitated for flue-cured tobacco grades of increasing stalk position using derivatization headspace solid-phase microextraction (SPME) with selected ion monitoring mode mass spectrometry. Qualitative analysis of the headspace of tobacco derivatized with methanolic hydrochloric acid using a 65-µm Carbowax–divinylbenzene SPME fiber indicates selectivity for relatively nonpolar volatile and semivolatile organic acid methyl esters. By contrast, direct exposure of an 85-µm polyacrylate SPME fiber to derivatives followed by GC–MS analysis provides the capability to evaluate significantly more polar organic acid methyl esters such as malic acid dimethylester and citric acid trimethylester.

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