Analysis of whiskey samples prepared
by a green microextraction
technique, dispersive liquid–liquid microextraction (DLLME),
before analysis by a qualitative gas chromatography–mass spectrometry
(GC/MS) method, is described as a laboratory experiment for an upper
division instrumental methods of analysis laboratory course. Here,
aroma compounds in whiskey samples (n = 11) were
extracted using ultrasound-assisted DLLME with chloroform (as extraction
solvent). The chloroform extract was analyzed by GC/MS with data manipulation
by AMDIS (automated mass spectral deconvolution and identification
system) to allow for comparisons between whiskey samples. Aroma compounds
commonly reported in the literature (furfural, isoamyl acetate, 5-methyl
furfural, ethyl esters, phenylethyl alcohol, whiskeylactone, and vanillin)
were tentatively identified based upon the match to the MS library.
This unique laboratory allows students to engage in a real-world analysis
of a high-value product and to explore the use of AMDIS to tentatively
identify compounds and compare chromatographic profiles of various
whiskey samples for identification of common and unique constituents.
Students also use the literature to provide sensory information for
these identified semivolatile compounds.
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