Analytical and Bioanalytical Chemistry

, Volume 411, Issue 10, pp 2031–2043 | Cite as

Carbon isotope compositions of whole wine, wine solid residue, and wine ethanol, determined by EA/IRMS and GC/C/IRMS, can record the vine water status—a comparative reappraisal

  • Jorge E. SpangenbergEmail author
  • Vivian Zufferey
Research Paper


Recently, we reported that the carbon isotope composition of the solid residues obtained by freeze-drying white and red wines (δ13CWSR) could be used for tracing the water status of the vines whose grapes were used to produce them. Here, we compare different methods using δ13C values of other wine components, particularly those of whole wine (δ13CWW) obtained by elemental analysis and isotope ratio mass spectrometry (EA/IRMS) and of wine ethanol (δ13CWEtOH) obtained by gas chromatography/combustion/IRMS (GC/C/IRMS), for their suitability to assess the vine water status. The studied wines were obtained from field-grown cultivars (Vitis vinifera L. cv. Chasselas, Petite Arvine, and Pinot noir) under different water treatments during the 2009–2014 seasons and were the same wines in which the δ13CWSR was measured previously. The EA/IRMS method for whole wine used two successive EA analytical cycles in each acquisition period to reduce the residence time of the sample capsules in the autosampler. The sample aliquots for the EA/IRMS and GC/C/IRMS analyses were optimized for peak-size differences less than 10% between the sample and reference gas. For all wine varieties, the δ13CWW and δ13CWEtOH values were linearly correlated with the predawn leaf water potential (Ψpd) and therefore serve as reliable indicators of vine water status, as do the δ13C values for must sugars and wine solid residues. The strongest negative correlations with Ψpd were for δ13Csugars (r = −0.94, n = 54) and δ13CWEtOH (r = −0.91) and were lower but still highly significant (p < 0.00001) for δ13CWW (r = −0.71) and δ13CWSR (r = −0.70). An evaluation of the advantages and drawbacks of the different methods is presented, showing that the δ13C analysis of wine ethanol by GC/C/IRMS is the most appropriate.


Carbon isotope ratio δ13C value Vine water status Whole wine Wine ethanol Wine solid residue 



The stable isotope facilities were funded by the University of Lausanne. The authors are very grateful to Fabrice Forenzini and Johannes Rösti for providing bottles of Leytron wines and a standard aqueous solution of wine-derived ethanol.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflicts of interest.

Ethical approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Supplementary material

216_2019_1625_MOESM1_ESM.pdf (176 kb)
ESM 1 (PDF 139 kb)


  1. 1.
    Rossmann A, Schmidt HL, Reniero F, Versini G, Moussa I, Merle MH. Stable carbon isotope content in ethanol of EC data bank wines from Italy, France and Germany. Z Lebensm Unters Forsch. 1996;203:293–301.CrossRefGoogle Scholar
  2. 2.
    Spangenberg JE, Macko SA, Hunziker J. Characterization of olive oil by carbon isotope analysis of individual fatty acids: implications for authentication. J Agric Food Chem. 1998;46:4179–84.CrossRefGoogle Scholar
  3. 3.
    Ogrinc N, Kosir IJ, Spangenberg JE, Kidrić J. The application of NMR and MS methods for detection of adulteration of wine, fruit juices, and olive oil. A review. Anal Bioanal Chem. 2003;376:424–30.CrossRefPubMedGoogle Scholar
  4. 4.
    Richter EK, Spangenberg JE, Kreuzer M, Leiber F. Characterization of rapeseed (Brassica napus) oils by bulk C, O, H, and fatty acid C stable isotope analyses. J Agric Food Chem. 2010;58:8048–55.CrossRefPubMedGoogle Scholar
  5. 5.
    Spangenberg JE. Bulk C, H, O, and fatty acid C stable isotope analyses for purity assessment of vegetable oils from the southern and northern hemispheres. Rapid Commun Mass Spectrom. 2016;30:2247–461.CrossRefGoogle Scholar
  6. 6.
    O’Neill BC, Oppenheimer M, Warren R, Hallegatte S, Kopp RE, Portner HO, et al. IPCC reasons for concern regarding climate change risks. Nat Clim Chang. 2017;7:28–37.CrossRefGoogle Scholar
  7. 7.
    van Leeuwen C, Tregoat O, Chone X, Bois B, Pernet D, Gaudillère JP. Vine water status is a key factor in grape ripening and vintage quality for red Bordeaux wine. How can it be assessed for vineyard management purposes? I Int Sci Vigne Vin. 2009;43:121–34.Google Scholar
  8. 8.
    Pagay V, Zufferey V, Lakso AN. The influence of water stress on grapevine (Vitis vinifera L.) shoots in a cool, humid climate: growth, gas exchange and hydraulics. Funct Plant Biol. 2016;43:827–37.CrossRefGoogle Scholar
  9. 9.
    Medrano H, Escalona JM, Bota J, Gulias J, Flexas J. Regulation of photosynthesis of C-3 plants in response to progressive drought: stomatal conductance as a reference parameter. Ann Bot. 2002;89:895–905.CrossRefPubMedPubMedCentralGoogle Scholar
  10. 10.
    Farquhar GD, Ehleringer JR, Hubick KT. Carbon isotope discrimination and photosynthesis. Annu Rev Plant Physiol Plant Mol Biol. 1989;40:503–37.CrossRefGoogle Scholar
  11. 11.
    Gaudillère JP, van Leeuwen C, Ollat N. Carbon isotope composition of sugars in grapevine, an integrated indicator of vineyard water status. J Exp Bot. 2002;53:757–63.CrossRefPubMedGoogle Scholar
  12. 12.
    Chone X, van Leeuwen C, Dubourdieu D, Gaudillere JP. Stem water potential is a sensitive indicator of grapevine water status. Ann Bot. 2001;87:477–83.CrossRefGoogle Scholar
  13. 13.
    de Souza CR, Maroco JP, dos Santos TP, Rodrigues ML, Lopes CM, Pereira JS, et al. Impact of deficit irrigation on water use efficiency and carbon isotope composition (delta C-13) of field-grown grapevines under Mediterranean climate. J Exp Bot. 2005;56:2163–72.CrossRefPubMedGoogle Scholar
  14. 14.
    van Leeuwen C, Tregoat O, Pernet D, Roby JP, Cellie N, Gaudillère JP. Use of sarbon isotope discrimination on grape sugar as a tool for practical vineyard management. Am J Enol Vitic. 2009;60:394A.Google Scholar
  15. 15.
    Jackson RS. Wine science. Principles and applications. New York: Elsevier/Academic Press; 2014.Google Scholar
  16. 16.
    Breda N, Granier A, Barataud F, Moyne C. Soil water dynamics in an oak stand. I. Soil moisture, water potentials and water uptake by roots. Plant Soil. 1995;172:17–27.CrossRefGoogle Scholar
  17. 17.
    Pellegrino A, Lebon E, Simonneau T, Wery J. Towards a simple indicator of water stress in grapevine (Vitis vinifera L.) based on the differential sensitivities of vegetative growth components. Aust J Grape Wine Res. 2005;11:306–15.CrossRefGoogle Scholar
  18. 18.
    Guyon F, van Leeuwen C, Gaillard L, Grand M, Akoka S, Remaud GS, et al. Comparative study of 13C composition in ethanol and bulk dry wine using isotope ratio monitoring by mass spectrometry and by nuclear magnetic resonance as an indicator of vine water status. Anal Bioanal Chem. 2015;407:9053–60.CrossRefPubMedGoogle Scholar
  19. 19.
    Spangenberg JE, Vogiatzaki M, Zufferey V. Gas chromatography and isotope ratio mass spectrometry of Pinot noir wine volatile compounds (δ 13C) and solid residues (δ 13C, δ 15N) for the reassessment of vineyard water-status. J Chromatogr A. 2017;1517:142–55.CrossRefPubMedGoogle Scholar
  20. 20.
    Zufferey V, Spring JL, Verdenal T, Dienes A, Belcher S, Lorenzini F, et al. Influence of water stress on plant hydraulics, gas exchange, berry composition and quality of Pinot noir wines in Switzerland. OENO One. 2017;51:37–57.CrossRefGoogle Scholar
  21. 21.
    Spangenberg JE, Zufferey V. Changes in soil water availability in vineyards can be traced by the carbon and nitrogen isotope composition of dried wines. Sci Total Environ. 2018;635:178–87.CrossRefPubMedGoogle Scholar
  22. 22.
    Cabañero AI, Recio JL, Ruperez M. Isotope ratio mass spectrometry coupled to liquid and gas chromatography for wine ethanol characterization. Rapid Commun Mass Spectrom. 2008;22:3111–8.CrossRefPubMedGoogle Scholar
  23. 23.
    Spitzke ME, Fauhl-Hassek C. Determination of the 13C/12C ratios of ethanol and higher alcohols in wine by GC-C-IRMS analysis. Eur Food Res Technol. 2010;231:247–57.CrossRefGoogle Scholar
  24. 24.
    Coplen TB. Guidelines and recommended terms for expression of stable-isotope-ratio and gas-ratio measurement results. Rapid Commun Mass Spectrom. 2011;25:2538–60.CrossRefPubMedGoogle Scholar
  25. 25.
    Brand WA. New reporting guidelines for stable isotopes – an announcement to isotope users. Isot Environ Health Stud. 2011;47:535–6.CrossRefGoogle Scholar
  26. 26.
    Schimmelmann A, Qi HP, Coplen TB, Brand WA, Fong J, Meier-Augenstein W, et al. Organic reference materials for hydrogen, carbon, and nitrogen stable isotope-ratio measurements: caffeines, n-alkanes, fatty acid methyl esters, glycines, L-valines, polyethylenes, and oils. Anal Chem. 2016;88:4294–302.CrossRefPubMedGoogle Scholar
  27. 27.
    Bruno TJ, Lide DR, Rumble JR, editors. CRC handbook of chemistry and physics, 99th edn (Internet Version). Boca Raton: CRC Press; 2018.Google Scholar
  28. 28.
    Bisson LF, Joseph CML. Yeasts. In: König H, Unden G, Fröhlich J, editors. Biology of microorganisms on grapes, in must and in wine. Berlin-Heidelberg: Springer; 2009. p. 47–60.CrossRefGoogle Scholar
  29. 29.
    Rossmann A, Butzenlechner M, Schmidt HL. Evidence for a non-statistical carbon isotope distribution in natural glucose. Plant Physiol. 1991;96:609–14.CrossRefPubMedPubMedCentralGoogle Scholar
  30. 30.
    Hobbie EA, Werner RA. Intramolecular, compound-specific, and bulk carbon isotope patterns in C3 and C4 plants: a review and synthesis. New Phytol. 2004;161:371–85.CrossRefGoogle Scholar
  31. 31.
    Pretorius IS. Tailoring wine yeast for the new millennium: novel approaches to the ancient art of winemaking. Yeast. 2000;16:675–729.CrossRefPubMedGoogle Scholar
  32. 32.
    Bayle K, Akoka S, Remaud GS, Robins RJ. Nonstatistical 13C distribution during carbon transfer from glucose to ethanol during fermentation is determined by the catabolic pathway exploited. J Biol Chem. 2015;290:4118–28.CrossRefPubMedGoogle Scholar
  33. 33.
    Gilbert A, Silvestre V, Segebarth N, Tcherkez G, Guillou C, Robins RJ, et al. The intramolecular 13C-distribution in ethanol reveals the influence of the CO2-fixation pathway and environmental conditions on the site-specific 13C variation in glucose. Plant Cell Environ. 2011;34:1104–12.CrossRefPubMedGoogle Scholar
  34. 34.
    Waterhouse AL. Elias RJ (2010) chemical and physical deterioration of wine. In: Skibsted LH, Risbo J, Andersen ML, editors. Chemical deterioration and physical instability of food and beverages. Cambridge: Woodhead; 2010. p. 466–82.CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Institute of Earth Surface Dynamics (IDYST)University of LausanneLausanneSwitzerland
  2. 2.Institute of Plant Production Sciences Agroscope, Viticulture Research CenterPullySwitzerland

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