Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings

Câmara, J. S.; Marques, J. C.; Perestrelo, Rosa Maria de Sá; Rodrigues, F.; Oliveira, L.; Andrade, P.; Caldeira, M.

http://hdl.handle.net/10400.13/904

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Authors

Câmara, J. S.

Marques, J. C.

Perestrelo, Rosa Maria de Sá

Abstract(s)

A dynamic headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to ion trap mass spectrometry (GC–ITMS) method was developed and applied for the qualitative determination of the volatile compounds present in commercial whisky samples which alcoholic content was previously adjusted to 13% (v/v). Headspace SPME experimental conditions, such as ﬁbre coating, extraction temperature and extraction time, were optimized in order to improve the extraction process. Five different SPME ﬁbres were used in this study, namely, poly(dimethylsiloxane)(PDMS),poly(acrylate)(PA),Carboxen-poly(dimethylsiloxane)(CAR/PDMS),Carbowax-divinylbenzene(CW/DVB)and Carboxen-poly(dimethylsiloxane)-divinylbenzene (CAR/PDMS/DVB). The best results were obtained using a 75 m CAR/PDMS ﬁbre during headspace extraction at 40◦C with stirring at 750rpm for 60min, after saturating the samples with salt. The optimised methodology was then appliedtoinvestigatethevolatilecompositionproﬁleofthreeScotchwhiskysamples—BlackLabel,BallantinesandHighlandClan.Approximately seventy volatile compounds were identiﬁed in the these samples, pertaining at several chemical groups, mainly fatty acids ethyl esters, higher alcohols, fatty acids, carbonyl compounds, monoterpenols, C13 norisoprenoids and some volatile phenols. The ethyl esters form an essential group of aroma components in whisky, to which they confer a pleasant aroma, with “fruity” odours. Qualitatively, the isoamyl acetate, with “banana” aroma,wasthemostinteresting.Quantitatively,signiﬁcantcomponentsareethylestersofcaprilic,capricandlauricacids.Thehighestconcentration of fatty acids, were observed for caprilic and capric acids. From the higher alcohols the fusel oils (3-methylbutan-1-ol and 2.phenyletanol) are the most important ones.

Keywords

Whisky analysis Headspace solid phase microextraction (HS-SPME) Volatile compounds Gas chromatography–Mass spectrometry (GC–MS) . Faculdade de Ciências Exatas e da Engenharia

URI

http://hdl.handle.net/10400.13/904

Citation

Câmara, J. S., Marques, J. C., Perestrelo, R. M., Rodrigues, F., Oliveira, L., Andrade, P., & Caldeira, M. (2007). Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings. Journal of Chromatography a, 1150(1), 198-207.