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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.

Derivatization Solid-Phase Microextraction Gas Chromatographic—Mass Spectrometric Determination of Organic Acids in Tobacco