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Wine Authenticity by Quantitative 1H NMR Versus Multitechnique Analysis: a Case Study

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Wine Authenticity by Quantitative 1H NMR Versus Multitechnique Analysis: a Case Study Wine Authenticity by Quantitative 1H NMR Versus Multitechnique Analysis: a Case Study Louis Gougeon, Gregory da Costa, Tristan Richard & François Guyon Food Analytical Methods ISSN 1936-9751 Volume 12 Number 4 Food Anal. Methods (2019) 12:956-965 DOI 10.1007/s12161-018-01425-z 1 23 Your article is protected by copyright and all rights are held exclusively by Springer Science+Business Media, LLC, part of Springer Nature. This e-offprint is for personal use only and shall not be self-archived in electronic repositories. If you wish to self- archive your article, please use the accepted manuscript version for posting on your own website. You may further deposit the accepted manuscript version in any repository, provided it is only made publicly available 12 months after official publication or later and provided acknowledgement is given to the original source of publication and a link is inserted to the published article on Springer's website. The link must be accompanied by the following text: "The final publication is available at link.springer.com”. 1 23 Author's personal copy Food Analytical Methods (2019) 12:956–965 https://doi.org/10.1007/s12161-018-01425-z Wine Authenticity by Quantitative 1H NMR Versus Multitechnique Analysis: a Case Study Louis Gougeon 1 & Gregory da Costa1 & Tristan Richard1 & François Guyon2 Received: 27 September 2018 /Accepted: 26 December 2018 /Published online: 15 January 2019 # Springer Science+Business Media, LLC, part of Springer Nature 2019 Abstract Food counterfeit is a major issue for food industries. In the case of wines, there can be multiple forgeries such as geographical, vintage, or varietal mislabeling. For the last 10 years, the use of quantitative 1H NMR (q-NMR) for food authentication has experienced an enormous increase. This study was based on a comparative evaluation of the results obtained for three sets of authentic high-valued wines and suspected wines. Two methodologies have been followed: (i) the usual wine analysis, based on the utilization of multiple techniques, which is the traditional way of analysis for wine authentication and (ii) q-NMR profiling, the alternative proposed method. For wine comparison, an original approach based on similarity score (S-score) by analogy to the Z-score calculation was developed. A limit of four S-scores outside the range − 2/2 has been, arbitrary, defined to reveal that wines are different using q-NMR analysis. Data treatments allowed the extraction of discriminating parameters, some of which were common to both approaches while others could be linked to the techniques’ capabilities showing the complementarity of the two approaches. This study demonstrated the potential of q-NMR in wine authentication by comparative analysis with authentic samples. The q-NMR alternative method has also the advantages of rapidity (around 20 min including sample preparation, analysis, and data treatment) and low volume (0.5 mL), which is a prerequisite for analyzing priceless wines. Keywords Food authenticity . Food quality control . Wine . Classical wine analysis . 1HNMR . q-NMR . Chemometric Introduction using various analytical (Schlesier et al. 2009;Medina et al. 2013) and statistical methods (Smeyers-Verbeke et Food authenticity is a major concern in the global food al. 2009). Multi-instrumental approaches have been used system for many reasons such as safety, consumer trust, including liquid and gas chromatography, UV-visible spec- and producer concurrency. Falsifications occurring in wine trometry, near-infrared spectrometry, NMR, mass spec- can belong to multiple types including geographical, vin- trometry (MS), isotope ratio mass spectrometry (IRMS), tage, and varietal mislabeling. The detection of such falsi- and coupled plasma mass spectroscopy (ICP-MS). All fications is usually performed using the confrontation of these techniques are widely employed in the investigation analytical results between authentic and suspicious wines of wine authenticity allowing the measurement of several wine parameters such as ethanol and alcohols, sulfur diox- ide, reducing sugars, polyphenols, organic acids, total and Electronic supplementary material The online version of this article volatile acidity, minerals, metals, and isotopic ratios (D/H, 18 16 13 12 (https://doi.org/10.1007/s12161-018-01425-z) contains supplementary O/ O, C/ C). Until now, all these multidisciplinary material, which is available to authorized users. approaches are necessary to obtain discriminant results (so-called in this paper usual wine analysis) (Medina * François Guyon et al. 2013). As a result, wine authenticity study requires [email protected] highly skilled technicians, numerous analytical systems, and a large volume of wine. The overall analysis can take 1 Univ. Bordeaux, ISVV, EA 4577, USC 1366 INRA, Unité de Recherche, Œnologie, 210 Chemin de Leysotte, 33882 Villenave time and is costly. The NMR quantitative analysis (q- d’Ornon, France NMR) could be a complementary alternative to the usual 2 Service Commun des Laboratoires, 3 Avenue du Dr. Albert wine analysis because it can be considered as a universal Schweitzer, 33600 Pessac, France method that allows the measurement of several parameters Author's personal copy Food Anal. Methods (2019) 12:956–965 957 on a small volume of wine without specific sample prepa- treatment will compare analytical information provided by ration procedure (Pauli et al. 2012). these two different approaches in order to evaluate q-NMR Since 10 years, 1H NMR analysis has been more and more potential in wine authentication by comparative data analysis widely applied to food control and, as a result, to wine (Larive of suspicious and authentic wines. et al. 2014; Simmler et al. 2014; Amargianitaki and Spyros 2017). The application of proton profiling or compound quan- tification obtained by q-NMR along with chemometrics has Material and Methods been successfully used for recognizing grape varieties (Son et al. 2009a, b; Anastasiadi et al. 2009; Godelmann et al. Samples 2013), geographical origin (Caruso et al. 2012; Viggiani and Castiglione Morelli 2008; Son et al. 2008; Pereira et al. 2007) In order to respect the anonymity, three sets of samples were and vintage (Consonni et al. 2011). The q-NMR interest identified as A, B, and C, corresponding to three different comes from the global analysis of the food matrix, the repeat- vintages, one old (A, prior to the 2000 vintage) and two youn- ability and reproducibility of the measurements as well as its ger ones (B and C). The first set of samples was composed of rapidity in comparison to classical methods (Godelmann et al. two bottles (As1 and As2) which are expected to be used for top 2016). up leveling. The second set of samples, corresponding to sus- High-value wines are to be kept for aging, and, sometimes, picious bottles found on the market, was based on a single some of them become wines of collection. Authenticity as- bottle for each of the two vintages (Bs and Cs). For each sessment and good conservation of these wines are thus crit- vintage, Château Mouton Rothschild provided a bottle of the ical questions. On one hand, greed and profit could lead un- authentic wine of their own cellar identified as Aa,Ba,andCa. scrupulous resellers to practice wine forgeries (geographical, In addition, Château Mouton Rothschild provided three sets of vintage, or varietal mislabeling) on such priceless wines. On authentic bottles from different old vintages (prior to the 1980 the other hand, during long-aging period, corks can dry out vintage) identified as vintages N, N +2,andN + 4 (5, 4, and 4 due to a lack of humidity which, in addition to wine leak, bottles, respectively). induces oxygen exchanges causing wine spoilage or oxida- To validate the 1H NMR wine analysis method, 20 French tion. As a result, these two aspects become critical for driving wines were purchased commercially: a set of 13 wines from an early wine degradation. The unique solution is to replace South-West region (6 Médoc, 6 Libournais, and 1 Gascogne), the cork and to top the bottle up with a similar wine, i.e., same a set of 4 wines from Burgundy region (2 Burgundy and 2 vintage and same production estate. The wine producer is the Beaujolais), 2 Loire Valley wines, and 1 Roussillon wine only one licensed to perform this top-up level step which is (Table S1, supplementary data). realized after a control of wine authenticity. For both applica- tions, vineyard estates are searching for reliable authentication Usual Wine Analysis Methods techniques requiring the lowest sample volume to be used for analysis. Among q-NMR advantages, a valuable one is the All these analyses were performed strictly following the offi- low quantity of sample required for the analysis (Gougeon cial methods internationally recognized and referenced in the et al. 2018). As a result, this tool can be interesting in old Organisation Internationale de la Vigne et du Vin (OIV) com- vintage wine authentication using proton profile comparison pendium: alcoholic strength (ethanol) [OIV a], sugars (glu- between the authentic estate wine and the commercial one. cose, fructose, sucrose, glycerol) [OIV b], acidity (total and But until now, q-NMR has not been applied for authentication volatile acidity) [OIV c], volatile compounds (ethanal, ethyl applications using the wine proton profile comparison. acetate, methanol, butanol 2, propanol 1) [OIV d], organic Recently, in collaboration with Château Mouton acid concentration (tartaric, malic, succinic, lactic and Rothschild, a prestigious winemaker, the authenticity of dif- gluconic acids) by high pressure capillary electrophoresis ferent wines samples was checked using the q-NMR method (HPCE) [OIV e], metal and trace metal analysis by inductive and the usual analysis (multitechnique approach) applied for plasma atomic emission spectrometry (ICP-AES) [OIV f], wine authentication (Medina et al. 2013). The first case was ethanol deuterium analysis by 2H NMR ((D/H)1 and on the authentication of the wine contained in two bottles, half (D/H)2) [OIV g], ethanol and wine carbone-13 (written, re- filled, that would be used to top-up the level of one bottle.
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