Headspace solid-phase microextraction combined with mass spectrometry as a powerful analytical tool for proﬁling the terpenoid metabolomic pattern of hop-essential oil derived from Saaz variety

Gonçalves, João; Figueira, José S.; Rodrigues, Fátima; Câmara, José

http://hdl.handle.net/10400.13/948

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Headspace solid-phase microextraction combined with mass spectrometry as a powerful analytical tool for proﬁling the terpenoid metabolomic pattern of hop-essential oil derived from Saaz variety.pdf		896.57 KB	Adobe PDF	Download

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Abstract(s)

Hop(HumuluslupulusL.,Cannabaceaefamily)isprizedforitsessentialoilcontents,usedin beer production and, more recently, in biological and pharmacological applications. In this work,a methodinvolvingheadspace solid-phase microextractionand gas chromatography– mass spectrometry was developed and optimized to establish the terpenoid (monoterpenes and sesquiterpenes) metabolomic pattern of hop-essential oil derived from Saaz variety as a mean to explore this matrix as a powerful biological source for newer, more selective, biodegradable and naturally produced antimicrobial and antioxidant compounds. Different parameters affecting terpenoid metabolites extraction by headspace solid-phase microextraction were considered and optimized: type of ﬁber coatings, extraction temperature, extraction time, ionic strength, and sample agitation. In the optimized method, analytes were extracted for 30 min at 40 C in the sample headspace with a 50/30 m divinylbenzene/carboxen/polydimethylsiloxane coating ﬁber. The methodology allowed the identiﬁcation of a total of 27 terpenoid metabolites, representing 92.5% of the total Saaz hop-essential oil volatile terpenoid composition. The headspace composition was dominated by monoterpenes (56.1%, 13 compounds), sesquiterpenes (34.9%, 10), oxygenated monoterpenes (1.41%, 3), and hemiterpenes (0.04%, 1) some of which can probably contribute to the hop of Saaz variety aroma. Mass spectrometry analysis revealed that the main metabolites are the monoterpene -myrcene (53.0±1.1% of the total volatile fraction), and the cyclic sesquiterpenes, -humulene (16.6 ± 0.8%), and -caryophyllene (14.7 ± 0.4%), which together represent about 80% of the total volatile fraction from the hop-essential oil. Theseﬁndingssuggestthatthismatrixcanbeexploredasapowerfulbiosourceofterpenoid metabolites.

Keywords

Essential oil GC-qMS HopSaaz variety HS-SPME Terpenoid metabolites . Faculdade de Ciências Exatas e da Engenharia Centro de Química da Madeira

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http://hdl.handle.net/10400.13/948

Citation

Gonçalves, J., Figueira, J., Rodrigues, F., & Camara, J. S. (2012). Headspace solid‐phase microextraction combined with mass spectrometry as a powerful analytical tool for profiling the terpenoid metabolomic pattern of hop‐essential oil derived from Saaz variety. Journal of separation science, 35(17), 2282-2296.