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Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings.
J Chromatogr A. 2007 May 25; 1150(1-2):198-207.JC

Abstract

A dynamic headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to ion trap mass spectrometry (GC-(IT)MS) 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 microm CAR/PDMS fibre during headspace extraction at 40 degrees C with stirring at 750 rpm for 60 min, after saturating the samples with salt. The optimised methodology was then applied to investigate the volatile composition profile of three Scotch whisky samples--Black Label, Ballantines and Highland Clan. 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, was the most interesting. Quantitatively, significant components are ethyl esters of caprilic, capric and lauric acids. The highest concentration 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.

Authors+Show Affiliations

Centro de Química da Madeira, Departamento de Química, Universidade da Madeira, Campus Universitário da Penteada, 9000-390 Funchal, Portugal. jsc@uma.ptNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Comparative Study
Journal Article

Language

eng

PubMed ID

17027810

Citation

Câmara, J S., et al. "Comparative Study of the Whisky Aroma Profile Based On Headspace Solid Phase Microextraction Using Different Fibre Coatings." Journal of Chromatography. A, vol. 1150, no. 1-2, 2007, pp. 198-207.
Câmara JS, Marques JC, Perestrelo RM, et al. Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings. J Chromatogr A. 2007;1150(1-2):198-207.
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(1-2), 198-207.
Câmara JS, et al. Comparative Study of the Whisky Aroma Profile Based On Headspace Solid Phase Microextraction Using Different Fibre Coatings. J Chromatogr A. 2007 May 25;1150(1-2):198-207. PubMed PMID: 17027810.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings. AU - Câmara,J S, AU - Marques,J C, AU - Perestrelo,R M, AU - Rodrigues,F, AU - Oliveira,L, AU - Andrade,P, AU - Caldeira,M, Y1 - 2006/10/06/ PY - 2006/06/19/received PY - 2006/09/05/revised PY - 2006/09/06/accepted PY - 2006/10/10/pubmed PY - 2007/7/6/medline PY - 2006/10/10/entrez SP - 198 EP - 207 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1150 IS - 1-2 N2 - A dynamic headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to ion trap mass spectrometry (GC-(IT)MS) 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 microm CAR/PDMS fibre during headspace extraction at 40 degrees C with stirring at 750 rpm for 60 min, after saturating the samples with salt. The optimised methodology was then applied to investigate the volatile composition profile of three Scotch whisky samples--Black Label, Ballantines and Highland Clan. 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, was the most interesting. Quantitatively, significant components are ethyl esters of caprilic, capric and lauric acids. The highest concentration 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. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17027810/Comparative_study_of_the_whisky_aroma_profile_based_on_headspace_solid_phase_microextraction_using_different_fibre_coatings_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(06)01755-9 DB - PRIME DP - Unbound Medicine ER -