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

• Authors: Maria Metafa , Anastasios Economou
• Languages of publication: EN

Abstracts

EN

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. [...]

Keywords

EN

Primary volatile aroma compounds; Wine; Gas chromatography-mass spectrometry; Solid phase extraction; Validation

• Publisher: De Gruyter Open
• Journal: Open Chemistry
• Year: 2013
• Volume: 11
• Issue: 2
• Pages: 228-247

Dates

published

1 - 2 - 2013

online

29 - 11 - 2012

Contributors

author

Maria Metafa

author

Anastasios Economou

• Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Athens, 157 71, Greece

References

• [1] Y.Z. Günata, C. Bayonove, R. Baumes, R. Cordonnier, J. Chromatogr. 331, 83 (1985) http://dx.doi.org/10.1016/0021-9673(85)80009-1[Crossref]
• [2] E. Dimitriadis, P.J. Williams, Am. J. Enol. Viticult. 35, 66 (1984)
• [3] R. Flamini, J. Mass Spectrom. 40, 705 (2005) http://dx.doi.org/10.1002/jms.887[Crossref]
• [4] R. Cordonnier, C. Bayonove, Conn. Vigne Vin 15, 269 (1981)
• [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
• [6] S. Sell, A. Canbas, T. Cabaroglu, H. Erten, Z. Günata, Food Chem. 94, 319 (2006) http://dx.doi.org/10.1016/j.foodchem.2004.11.019[Crossref]
• [7] A. F. Pisarnitskii, Appl. Biochem. Microbiol. 37, 552 (2001) http://dx.doi.org/10.1023/A:1012390731145[Crossref]
• [8] A. Zalacain, J. Marín, G.L. Alonso, M.R. Salinas, Talanta 71, 1610 (2007) http://dx.doi.org/10.1016/j.talanta.2006.07.051[Crossref]
• [9] S. Maicas, J. Juan Mateo, Appl. Microbiol. Biotechnol. 67, 322 (2005) http://dx.doi.org/10.1007/s00253-004-1806-0[Crossref]
• [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.
• [11] I.L. Francis, M.A. Sefton, P.J. Williams, J. Sci. Food Agric. 59, 511 (1992) http://dx.doi.org/10.1002/jsfa.2740590414[Crossref]
• [12] N.A. Abbott, B.G. Coombe, P.J. Williams, Am. J. Enol. Viticult. 42, 167 (1991)
• [13] M.A. Sefton, I.L. Francis, P.J. Williams, J. Food Sci. 59, 142 (1994) http://dx.doi.org/10.1111/j.1365-2621.1994.tb06919.x[Crossref]
• [14] M.A. Sefton, Aust. J. Grape Wine Res. 4, 30 (1998) http://dx.doi.org/10.1111/j.1755-0238.1998.tb00132.x[Crossref]
• [15] M.A. Sefton, I.L. Francis, P.J. Williams, Am. J. Enol. Viticult. 44, 359 (1993)
• [16] M. Fernandez-Gonzalez, R. Di Stefano, A. Briones, Food Microbiol. 20, 35 (2003) http://dx.doi.org/10.1016/S0740-0020(02)00105-3[Crossref]
• [17] B.W. Zoecklein, J.E. Marcy, J.M. Williams, Y. Jasinski, J. Food Comp. Anal. 10, 55 (1997) http://dx.doi.org/10.1006/jfca.1996.0518[Crossref]
• [18] B.W. Zoecklein, C.H. Hackney, S.E. Duncan, J.E. Marcy, J. Ind. Microbiol. Biotechnol. 22, 100 (1999) http://dx.doi.org/10.1038/sj.jim.2900613[Crossref]
• [19] J.E. Sarry, Z. Günata, Food Chem. 87, 509 (2004) http://dx.doi.org/10.1016/j.foodchem.2004.01.003[Crossref]
• [20] T. Cabaroglu, S. Selli, A. Canbas, J.-P. Lepoutre, Z. Günata, Enzyme Microbial.Technol. 33, 581 (2003) http://dx.doi.org/10.1016/S0141-0229(03)00179-0[Crossref]
• [21] J.J. Mateo, J. Jimenez, J. Chromatogr. A 881, 557 (2000) http://dx.doi.org/10.1016/S0021-9673(99)01342-4[Crossref]
• [22] R.C. Ramón Natera, E. Durán, C. García-Barroso, Eur. Food. Res. Technol. 228, 1 (2008) http://dx.doi.org/10.1007/s00217-008-0900-4[Crossref]
• [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) http://dx.doi.org/10.1021/jf00049a023[Crossref]
• [24] J.J. Mateo, N. Gentilini, T. Huerta, M. Jimenez, R. Di Stefano, J. Chromatogr. A. 778, 219 (1997) http://dx.doi.org/10.1016/S0021-9673(97)00566-9[Crossref]
• [25] M. Esti, P. Tamborra, Anal. Chim. Acta 563, 173 (2006) http://dx.doi.org/10.1016/j.aca.2005.12.025[Crossref]
• [26] N. Carro, E. Lopez, Z.Y. Günata, R.L. Baumes, C.L. Bayonove, Analysis 24, 254 (1996)
• [27] R. López, M. Aznar, J. Cacho, V. Ferreira, J. Chromatogr. A 966, 167 (2002) http://dx.doi.org/10.1016/S0021-9673(02)00696-9[Crossref]
• [28] V. Ferreira, L. Ortega, A. Escudero, J.F. Cacho, J. Chromatogr. Sci. 38, 469 (2000) [Crossref]
• [29] Z. Piñeiro, M. Palma, C.G. Barroso, Anal. Chim. Acta 513, 209 (2004) http://dx.doi.org/10.1016/j.aca.2003.12.044[Crossref]
• [30] M. Dziadas, M. Nowacka, T. Jesionowski, H.H. Jelen, Anal. Chim. Acta 699, 66 (2011) http://dx.doi.org/10.1016/j.aca.2011.05.011[Crossref]
• [31] M.J. Ibarz, V. Ferreira, P. Hernandez-Orte, N. Loscos, J. Cacho, J. Chromatogr. A 1116, 217 (2006) http://dx.doi.org/10.1016/j.chroma.2006.03.020[Crossref]
• [32] L. Culleré, M. Aznar, J. Cacho, V. Ferreira, J. Chromatogr. A 1017, 17 (2003) http://dx.doi.org/10.1016/S0021-9673(03)01332-3[Crossref]
• [33] D. Hernanz, V. Gallo, A.F. Recamales, A.J. Meléndez-Martínez, F.J. Heredia, Talanta 76, 929 (2008) http://dx.doi.org/10.1016/j.talanta.2008.04.049[Crossref]
• [34] E. Sánchez-Palomo, M.E. Alañón, M.C. Díaz-Maroto, M.A. González-Viñas, M.S. Pérez-Coello, Talanta 79, 871 (2009) http://dx.doi.org/10.1016/j.talanta.2009.05.019[Crossref]
• [35] Guide to Quality in Analytical Chemistry: An Aid to Accreditation, 2002, CITAC and EURACHEM (http://www.eurachem.org/images/stories/Guides/pdf/CITAC_EURACHEM_GUIDE.pdf, assessed 31 October 2012)
• [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 (http://www.eurachem.org/images/stories/Guides/pdf/recovery.pdf, assessed 31 October 2012)
• [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 (http://www.sadcmet.org/SADCWaterLab/Reports/November%202006/at01_VAM.pdf, assessed 31 October 2012)
• [38] P. Lanaridis, M.J. Salaha, I. Tzourou, E. Tsoutsouras, S Karagiannis, J. Int. Sci. Vigne Vin 36, 39 (2002)
• [39] J.C.R. Demyttenaere, C. Dagher, P. Sandra, S. Kallithraka, R. Verhé, N. De Kimpe, J. Chromatogr. A, 985, 233 (2003) http://dx.doi.org/10.1016/S0021-9673(02)01467-X[Crossref]
• [40] S. Karagiannis, A. Economou, P. Lanaridis, J. Agric. Food Chem. 48, 5369 (2000) http://dx.doi.org/10.1021/jf000459c[Crossref]
• [41] R. Di Stefano, Bulletin de l’OIV 721, 219 (1991)
• [42] M. Vilanovaa, C. Sieiro, J. Food Comp. Anal. 19, 694 (2006) http://dx.doi.org/10.1016/j.jfca.2005.10.002[Crossref]
• [43] A.G. González, M. Ángeles Herrador, TrAC 26 227 (2007)
• [44] B.K. Matuszewski, M.L. Constanzer, C.M. Chavez-Eng, Anal. Chem. 75, 3019 (2003) http://dx.doi.org/10.1021/ac020361s[Crossref]
• [45] M. Sulyok, F. Berthiller, R. Krska, R. Schuhmacher, Rapid. Commun. Mass. Spectrom. 20, 2649 (2006) http://dx.doi.org/10.1002/rcm.2640[Crossref]
• [46] M. Thompson, Analyst 125, 2020 (2000) http://dx.doi.org/10.1039/b006376m[Crossref]
• [47] H.H. Jeleń, M. Majcher, M. Dziadas, R. Zawriska-Wojtasiak, K. Czaczyk, E. Wąsowicz, J. Chromatogr. A 1218, 7566 (2011) http://dx.doi.org/10.1016/j.chroma.2011.07.023[Crossref]
• [48] S.G. Voirin, R.L. Baumes, J.C. Sapis, C.L. Bayonove, J. Chromatogr. A 595, 269 (1992) http://dx.doi.org/10.1016/0021-9673(92)85169-T[Crossref]
• [49] J. Fenoll, A. Manso, P. Hellín, L. Ruiz, P. Flores, Food Chem. 114, 420 (2009) http://dx.doi.org/10.1016/j.foodchem.2008.09.060[Crossref]
• [50] E. Gómez García-Carpintero, E. Sánchez-Palomo, M.A. Gómez Gallego, M.A. González-Viñas, Food Chem. 131, 90 (2012) http://dx.doi.org/10.1016/j.foodchem.2011.08.035[Crossref]
• [51] D.A. Nagegowda, FEBS Lett. 584 2965 (2010)
• [52] J. Marais, S. Afr. J. Enol. Vitic. 4, 49 (1983)

Identifiers

DOI

10.2478/s11532-012-0154-7