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Use of Isotope Ratio Determination (13C/12C) to Assess the Production Method of Sparkling Wine

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Use of Isotope Ratio Determination (13C/12C) to Assess the Production Method of Sparkling Wine 338 CHIMIA 2016, 70, No. 5 Food Authenticity And AdulterAtion doi:10.2533/chimia.2016.338 Chimia 70 (2016) 338–344 © Swiss Chemical Society Use of Isotope Ratio Determination (13C/12C) to Assess the Production Method of Sparkling Wine Joël S. Rossier*, Valérie Maury, Laetitia Gaillard, and Elmar Pfammatter Abstract: The production of a sparkling wine can be performed with different methods taking from a few weeks to several years, which often justifies a difference in added value for the consumer. This paper presents the use of isotope ratio δ13C measurements combined with physico-chemical analyses for the determination of mislabelling of sparkling wines produced by ‘ancestral’, ‘traditional’, ‘closed tank’ or ‘gasification’ methods. This work shows that the isotope composition of CO compared with that of the corresponding dried residue of wine (DRW) can 2 assess whether carbonate CO in a sparkling wine originates from alcohol fermentation or from artificial gas 2 addition. Isotopic ratios expressed as δ 13C and δ 13C measurements have been obtained for each wine by CO2 DRW gasbench isotopic ratio mass spectroscopy and cavity ring down infrared spectroscopy, respectively. When the difference between δ 13C and δ 13C is negative, the presence of artificial CO can be undoubtedly inferred, CO2 DRW 2 which would exclude the production methods ‘ancestral’ or ‘traditional’ for instance. Other parameters such as alcohol content, sugar and acid distributions are also important to complete the analytical panel to aid fraud tracking. Keywords: Ancestral method · Closed tank · Isotopic ratio · Sparkling wine · Traditional method 1. Introduction bees. More recently, our laboratory has are able to track whether a producer is mis- introduced a method to determine the leading the consumer by mislabelling its Our laboratory has specialised on food δ13C of CO in sparkling drinks, including sparkling wine. 2 fraud detection by means of isotopic fin- sparkling water or wine by the gasbench Table 1 briefly summarises what is ger printing for the last 15 years. Different IRMS technique. Other laboratories have commonly expected for the different methods have been introduced based on used similar methods for δ13C analysis of production methods. ‘Ancestral’ method isotopic ratio mass spectrometry (IRMS) CO in ciders.[2] This article shows how this means that the sparkling wine is produced 2 including a method to detect the geograph- technology has been applied in the field of with minimal intervention; the addition of ical origin of fruit and vegetables grown in sparkling wine control and is an addition ‘liqueur de tirage’ or ‘liqueur d’expédi- Valais thanks to the isotopic ratio of 18O to other studies already performed on the tion’ (see Table 1 for an explanation of in the water fraction of those products.[1] authenticity of sparkling drinks using the the terminology; the French expressions In order to complete the scope of control, isotope ratio.[3–7] On the other hand, δ13C of are used throughout) is forbidden, which other kinds of analysis have been intro- the dried residue of wine (DRW) has also means that the whole wine carbon com- duced, based on the 13C/12C isotope ratio been developed in order to detect whether ponent should originate exclusively from δ13C. This parameter enables the integrity non-volatile wine components originate the grapes; furthermore, after a partial al- of natural products to be checked in case from grape or from chaptalisation (sugar coholic fermentation in a tank the cuvée of suspicion of addition of artificial ingre- addition to harvested grapes to increase the is bottled and further fermented until equi- dients; for instance the EA-IRMS meth- alcohol level) with cane sugar for example. librium is reached, stopping the fermenta- od has been used to determine whether a The latter application was implemented by tion at a relatively low alcoholic content honey has been adulterated by the addition cavity ring down IR spectroscopy (CRDS) (~7.5 % vol.). Once bottled, this wine is of cane sugar, either as a non-permitted instrumentation recently acquired in our fermented without transfer to a tank, ad- additive or as a feeding solution for the laboratory. dition or filtration steps; as a consequence Sparkling wines obtained by ‘ances- the residual sugar should exclusively come tral’ or ‘traditional’ methods are perceived from the grapes (no beet or cane sugar ad- as high value end products whereas in- dition), and the CO should only originate 2 dustrial sparkling wines, often produced from the fermentation of the grape sugar; in ‘closed tanks’ or simply ‘gasified’ are in addition these wines should not have found at very low prices in supermarkets. undergone malolactic fermentation. At These different methods reflect different the end of the fermentation, a disgorging costs of production as well as a strong dif- step is performed to remove most of the ferentiation for the consumer. It is clear yeast and other precipitate, but no filtra- that the label ‘traditional’ or ‘ancestral’ tion is performed during the production *Correspondence: Dr. J. S. Rossier method provides an added value which process. It has to be noted that some ex- Service de la consommation et des affaires vétéri- could lead to mislabelling. For the con- ception to these rules have been introduced naires (SCAV) sumer, it is impossible to detect this kind for the method ‘dioise ancestral’ for which Rue Pré d’Amédée 2 of fraud by simple degustation; therefore, a transfer to a closed tank together with a CH-1950 Sion E-mail: [email protected] it is important that food control authorities filtration is permitted.[8] Food Authenticity And AdulterAtion CHIMIA 2016, 70, No. 5 339 Table 1. Vinification processes of the different production methods. Ancestral Traditional Closed tank Gas addition Dioise alcoholic fermentation partial partial yes optional optional malolactic fermentation no no optional optional optional ‘liqueur de tirage’a addition no no yes optional no ‘in-bottle’ fermentation yes yes yes no no ‘in closed tank’ fermentation NAb NA NA yes no authorised artificial CO addition no no no no yes 2 ‘liqueur d’expédition’c addition no no optional optional optional disgorgingd yes no yes no no transfer in ‘cuve de tirage’noyes no yes yes filtration no yes no yes yes isobarometric ‘Tirage’e no yes no yes yes aLiqueur de tirage: solution containing yeast and sugar. Sugar can be C3 or C4. This solution is added when tranquil wine is transferred to the bottle or to the closed tank for the second alcoholic fermentation. bNot applicable. cLiqueur d’expédition: solution containing wine and sugar. Sugar can be C3 or C4. This solution is added after disgorging and determines which type of wine is produced (brut, sec, demi sec, doux). Quantity of sugar present in the solution defines the type of sparkling wine. dDisgorging describes a process that allows the elimination of a large part of residues present in bottle at the end of fermentation. This process substitutes filtration for some methods. Filtration eliminates all residues and the sparkling wine is totally limpid, disgorged sparkling wines retain some residue. e‘tirage isobarique’: This term is used when sparkling wine is transferred from tank to bottle. During this process, pressure is used to transfer wine from a closed tank into the bottle. This pressure is generally done by applying a flux of artificial CO . 2 Most famous sparkling wines such as ly from the in-bottle fermentation and not composed of four atoms of carbon. Grape Champagne or Cremant are produced by from any artificial source. vines, however, follow the C3 photosyn- the so-called ‘traditional’ method, which In order to decrease both the time thetic pathway in which the first organic is defined in the EU regulation 607/2009 and cost of sparkling wine production, molecule is composed of three atoms of as follows:[9] industrial methods such as ‘closed tank’ carbon. The stable carbon isotope ratios “The expressions ‘bottle-fermented fermentation are practiced. This consists (expressed as δ13C) of C4 and C3 plants by the traditional method’ or ‘traditional of a double-coated steel tank which can are significantly different, with δ13C val- method’ or ‘classical method’ or ‘classi- withstand pressure up to several bars. In ues for C4 plants varying from –11 to –14 cal traditional method’ may be used only these tanks, different sparkling wines can and those of C3 plants varying from –24 to describe sparkling wines with protected be produced, but in most of the cases, the to –32.[11] designations of origin or with a geograph- closed tank is filled with still wines sup- In order to track fraud and protect the ical indication of a third country or quality plemented with a ‘liqueur de tirage’ and consumer, exhaustive analyses of 30 dif- sparkling wines provided the product: fermented for two to three weeks. With ferent sparkling wines produced either by (a) was made sparkling by a second al- these industrial techniques, the tempera- ‘ancestral’, ‘ancestral dioise’, ‘tradition- coholic fermentation in the bottle; ture and pressure can be optimised in the al’, ‘closed tank’ and ‘gasified’ methods (b) stayed without interruption in con- closed tank to maximise the fermentation have been performed and reported in this tact with the lees for at least nine months in efficiency; after filtration, these sparkling work. Parameters such as δ13C of CO re- 2 the same undertaking from the time when wines are standardised and bottled with a veal whether the wine has been produced the cuvée was constituted; process called ‘tirage isobarique’. These exclusively in bottle, δ13C of the dried res- (c) was separated from the lees by dis- sparkling wines can be sold at a very com- idue of wine would tell whether cane sugar gorging.” petitive price compared to those produced has been added, whereas other parameters This definition means that the vinifica- with an ‘ancestral’ or ‘traditional’ method.
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