Skip to content
BY-NC-ND 3.0 license Open Access Published by De Gruyter Open Access November 29, 2012

Comparison of solid-phase extraction sorbents for the fractionation and determination of important free and glycosidically-bound varietal aroma compounds in wines by gas chromatography-mass spectrometry

Maria Metafa EMAIL logo and Anastasios Economou
From the journal Open Chemistry


A critical comparison was made of seven solid-phase extraction (SPE) sorbents for the fractionation and isolation of 21 important free and glycosidically-bound varietal volatile aroma compounds. The sample was subjected to SPE and the free aromatics were eluted with dichloromethane followed by elution of the glucoconjugates with methanol; after fractionation, the free fraction was analyzed directly by GC-MS while the sugar-bound fraction was enzymatically hydrolyzed to liberate the free compounds before analysis by GC-MS. The extraction efficiency for the free compounds was evaluated based on the analytes’ signal recovery and for the glycosidically-bound compounds in terms of the relative peak areas. The best results for both the free and bound fractions were obtained with the Isolute ENV+ resin. Following selection of the most efficient SPE material, a GC-MS method was validated (in terms of selectivity, linearity, limits of detection (LODs) and limits of quantification (LOQs), recovery, repeatability, within-laboratory reproducibility and uncertainty) for the quantitative determination of the free primary volatiles in white wines. Validation results are presented at 4 fortification levels (10, 50, 200 and 500 µL−1). Regarding linearity, the correlation coefficient of the matrix-matched calibration plots was ≥0.99 for all the compounds. The LOQs were in the range 0.6–17.5 µg L−1. Recoveries ranged from 61% to 120% while the% relative standard deviation of the within-laboratory reproducibility was in the range 1.3% to 17.7%. Finally, the% expanded uncertainty ranged from 3.1% to 40.3%. The method has been successfully applied to the analysis of 20 white wine samples.

[1] Y.Z. Günata, C. Bayonove, R. Baumes, R. Cordonnier, J. Chromatogr. 331, 83 (1985) in Google Scholar

[2] E. Dimitriadis, P.J. Williams, Am. J. Enol. Viticult. 35, 66 (1984) Search in Google Scholar

[3] R. Flamini, J. Mass Spectrom. 40, 705 (2005) in Google Scholar PubMed

[4] R. Cordonnier, C. Bayonove, Conn. Vigne Vin 15, 269 (1981) 10.20870/oeno-one.1981.15.4.1365Search in Google Scholar

[5] E. Fernández, S.M. Cortès, M. Castro, M. Gil, M.L. Gil de la Pena, in: A. Lonvaud-Fuel (Ed.), Oenologie 99, 6e Symposium International d’Oenologie, Bordeaux, June 1999, France (Tec & Doc, Paris 2000) 161 Search in Google Scholar

[6] S. Sell, A. Canbas, T. Cabaroglu, H. Erten, Z. Günata, Food Chem. 94, 319 (2006) in Google Scholar

[7] A. F. Pisarnitskii, Appl. Biochem. Microbiol. 37, 552 (2001) in Google Scholar

[8] A. Zalacain, J. Marín, G.L. Alonso, M.R. Salinas, Talanta 71, 1610 (2007) in Google Scholar PubMed

[9] S. Maicas, J. Juan Mateo, Appl. Microbiol. Biotechnol. 67, 322 (2005) in Google Scholar PubMed

[10] I.L. Francis, S. Kassara, A.C. Noble, P.J. Williams, In: A.L. Waterhouse, S.E. Ebeler (Eds.), Chemistry of Wine Flavour (American Chemical Society, Washington, DC, 1999) 13. 10.1021/bk-1998-0714.ch002Search in Google Scholar

[11] I.L. Francis, M.A. Sefton, P.J. Williams, J. Sci. Food Agric. 59, 511 (1992) in Google Scholar

[12] N.A. Abbott, B.G. Coombe, P.J. Williams, Am. J. Enol. Viticult. 42, 167 (1991) 10.1017/S0272503700094568Search in Google Scholar

[13] M.A. Sefton, I.L. Francis, P.J. Williams, J. Food Sci. 59, 142 (1994) in Google Scholar

[14] M.A. Sefton, Aust. J. Grape Wine Res. 4, 30 (1998) in Google Scholar

[15] M.A. Sefton, I.L. Francis, P.J. Williams, Am. J. Enol. Viticult. 44, 359 (1993) Search in Google Scholar

[16] M. Fernandez-Gonzalez, R. Di Stefano, A. Briones, Food Microbiol. 20, 35 (2003) in Google Scholar

[17] B.W. Zoecklein, J.E. Marcy, J.M. Williams, Y. Jasinski, J. Food Comp. Anal. 10, 55 (1997) in Google Scholar

[18] B.W. Zoecklein, C.H. Hackney, S.E. Duncan, J.E. Marcy, J. Ind. Microbiol. Biotechnol. 22, 100 (1999) in Google Scholar

[19] J.E. Sarry, Z. Günata, Food Chem. 87, 509 (2004) in Google Scholar

[20] T. Cabaroglu, S. Selli, A. Canbas, J.-P. Lepoutre, Z. Günata, Enzyme Microbial.Technol. 33, 581 (2003) in Google Scholar

[21] J.J. Mateo, J. Jimenez, J. Chromatogr. A 881, 557 (2000) in Google Scholar

[22] R.C. Ramón Natera, E. Durán, C. García-Barroso, Eur. Food. Res. Technol. 228, 1 (2008) in Google Scholar

[23] P.J. Williams, W. Cynkar, I.L. Francis, J.D. Gray, P.G. Iland, B.G. Coombe, J. Agric. Food Chem. 43, 121 (1995) in Google Scholar

[24] J.J. Mateo, N. Gentilini, T. Huerta, M. Jimenez, R. Di Stefano, J. Chromatogr. A. 778, 219 (1997) in Google Scholar

[25] M. Esti, P. Tamborra, Anal. Chim. Acta 563, 173 (2006) in Google Scholar

[26] N. Carro, E. Lopez, Z.Y. Günata, R.L. Baumes, C.L. Bayonove, Analysis 24, 254 (1996) Search in Google Scholar

[27] R. López, M. Aznar, J. Cacho, V. Ferreira, J. Chromatogr. A 966, 167 (2002) in Google Scholar

[28] V. Ferreira, L. Ortega, A. Escudero, J.F. Cacho, J. Chromatogr. Sci. 38, 469 (2000) 10.1093/chromsci/38.11.469Search in Google Scholar

[29] Z. Piñeiro, M. Palma, C.G. Barroso, Anal. Chim. Acta 513, 209 (2004) in Google Scholar

[30] M. Dziadas, M. Nowacka, T. Jesionowski, H.H. Jelen, Anal. Chim. Acta 699, 66 (2011) in Google Scholar

[31] M.J. Ibarz, V. Ferreira, P. Hernandez-Orte, N. Loscos, J. Cacho, J. Chromatogr. A 1116, 217 (2006) in Google Scholar

[32] L. Culleré, M. Aznar, J. Cacho, V. Ferreira, J. Chromatogr. A 1017, 17 (2003) in Google Scholar

[33] D. Hernanz, V. Gallo, A.F. Recamales, A.J. Meléndez-Martínez, F.J. Heredia, Talanta 76, 929 (2008) in Google Scholar PubMed

[34] E. Sánchez-Palomo, M.E. Alañón, M.C. Díaz-Maroto, M.A. González-Viñas, M.S. Pérez-Coello, Talanta 79, 871 (2009) in Google Scholar PubMed

[35] Guide to Quality in Analytical Chemistry: An Aid to Accreditation, 2002, CITAC and EURACHEM (, assessed 31 October 2012) Search in Google Scholar

[36] M. Thompson, S.L.R. Ellison, A. Fajgelj, P. Willetts, R. Wood, Harmonised Guidelines for the Use of Recovery Information in Analytical Measurement, (Technical Report), 1996 (, assessed 31 October 2012) Search in Google Scholar

[37] V.J. Barwick, S.L.R Ellison, Part (d): Protocol for Uncertainty Evaluation from Validation Data, 2000 Report No: LGC/VAM/1998/088LGC/VAM/1998/088, Version 5.1 (, assessed 31 October 2012) Search in Google Scholar

[38] P. Lanaridis, M.J. Salaha, I. Tzourou, E. Tsoutsouras, S Karagiannis, J. Int. Sci. Vigne Vin 36, 39 (2002) 10.20870/oeno-one.2002.36.1.981Search in Google Scholar

[39] J.C.R. Demyttenaere, C. Dagher, P. Sandra, S. Kallithraka, R. Verhé, N. De Kimpe, J. Chromatogr. A, 985, 233 (2003) in Google Scholar

[40] S. Karagiannis, A. Economou, P. Lanaridis, J. Agric. Food Chem. 48, 5369 (2000) in Google Scholar

[41] R. Di Stefano, Bulletin de l’OIV 721, 219 (1991) Search in Google Scholar

[42] M. Vilanovaa, C. Sieiro, J. Food Comp. Anal. 19, 694 (2006) in Google Scholar

[43] A.G. González, M. Ángeles Herrador, TrAC 26 227 (2007) 10.1016/j.trac.2007.01.009Search in Google Scholar

[44] B.K. Matuszewski, M.L. Constanzer, C.M. Chavez-Eng, Anal. Chem. 75, 3019 (2003) in Google Scholar

[45] M. Sulyok, F. Berthiller, R. Krska, R. Schuhmacher, Rapid. Commun. Mass. Spectrom. 20, 2649 (2006) in Google Scholar

[46] M. Thompson, Analyst 125, 2020 (2000) in Google Scholar

[47] H.H. Jeleń, M. Majcher, M. Dziadas, R. Zawriska-Wojtasiak, K. Czaczyk, E. Wąsowicz, J. Chromatogr. A 1218, 7566 (2011) in Google Scholar

[48] S.G. Voirin, R.L. Baumes, J.C. Sapis, C.L. Bayonove, J. Chromatogr. A 595, 269 (1992) in Google Scholar

[49] J. Fenoll, A. Manso, P. Hellín, L. Ruiz, P. Flores, Food Chem. 114, 420 (2009) in Google Scholar

[50] E. Gómez García-Carpintero, E. Sánchez-Palomo, M.A. Gómez Gallego, M.A. González-Viñas, Food Chem. 131, 90 (2012) in Google Scholar

[51] D.A. Nagegowda, FEBS Lett. 584 2965 (2010) 10.1016/j.febslet.2010.05.045Search in Google Scholar PubMed

[52] J. Marais, S. Afr. J. Enol. Vitic. 4, 49 (1983) 10.1080/00362176685190131Search in Google Scholar

Published Online: 2012-11-29
Published in Print: 2013-2-1

© 2013 Versita Warsaw

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Downloaded on 27.1.2023 from
Scroll Up Arrow