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Ciência Téc. Vitiv. 21 (2), 53-65. 2006

2,4,6-TRICHLOROANISOLE: A CONSUMER PANEL

EVALUATION

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1

Faculdade de Farmácia da Universidade de Lisboa, Av. das Forças Armadas, 1649-019 Lisboa, Portugal

2

Instituto de Tecnologia Química e Biológica, Apartado 127, 2784-505 Oeiras, Portugal

3

Estação Vitivinícola Nacional (INIAP), 2565-191 Dois Portos, Portugal

4

Instituto de Biologia Experimental e Tecnológica, Apartado 12, 2781-901, Oeiras, Portugal

5

Instituto Superior Técnico, Av. Rovisco Pais, 1049-001 Lisboa, Portugal

*Corresponding author. Tel: +351214469770; fax: +351214417062, E-mail address: [email protected]

(Manuscrito recebido em 11.07.06. Aceite para publicação em 23.12.06)

SUMMARY

The “cork taint” is a major problem in wine industry and may caused by the several sources of contamination although wine cork stoppers are usually subject to suspition: 2,4,6-trichloroanisole (TCA) has been frequently associated to this off-flavour.

In this work, a consumer panel performed “forced choice” triangular tests in order to measure Odour Detection Thresholds (ODT) and Taste Detection Thresholds (TDT) of TCA in water, hydro-alcoholic solutions (11.5% and 18% ethanol) and white and red wines.

A paired preference test was also performed by the panel in order to measure Odour Rejection Threshold (ORT) in white and red wines spiked with TCA.

Results obtained show that the ODT and the TDT for TCA were respectively: 0.2 and 0.3 ng/ L in water, 0.9 and 1.7 ng/L in red wine and 1.5 and 1.0 ng/L in white wine. ODT were 4 and 10 ng/L respectively for hydro-alcoholic solutions with 11.5% and 18% ethanol. ORT for white wines was 10.4 ng/L and for red wines 16.0 ng/L.

These results suggest that although this group of non trained assessors detected very low concentrations of TCA in wines, they did not reject the wine at these low concentration values.

Key words: TCA; Cork taint; wine; sensory evaluation

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MATERIALS AND METHODS

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binomial distribution for triangular tests for the ODT (N = 44) and the TDT (N = 32) determination

Proporção cumulativa do número de consumidores que identificou correctamente o vinho branco contaminado com TCA para cada concentração testada para a determinação do LDO (----) e LDG (¯ ). A linha a 0,33 representa a proporção de resultados obtidos por resposta alietória; as linhas 0,48 e 0,5 indicam para o LDO (N = 44) e o LDG (N = 32)

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TABLE I

Threshold values for TCA (concentration in ng/L) accessed in different matrices. ODT: odour detection threshold; TDT: taste detection threshold; ORT: odour rejection threshold;

N: number of assessors; n.p.: not performed.

Limiares determinados para o TCA (concentração em ng/L) em diferentes matrizes. LDO: limiar de detecção olfactivo; LDG: limiar de detecção gustativo; LRO: limiar de rejeição

olfactivo, N- número total de consumidores; n.p.- teste não efectuado

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ORT using the binomial distribution for a paired two-sided test (N = 26)

Proporção cumulativa do número de consumidores que escolheu o vinho branco sem adição de TCA, para cada valor de concentração estudado. A linha a 0,5 representa os resultados obtidos por resposta alietória e a linha a 0,73 indica para o LRO a proporção de resultados a obter para um critério de significância dos resultados de 5% considerando

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RESUMO

2,4,6-Tricloroanisol: avaliação por um painel de consumidores

O denominado “gosto a rolha” é um problema de grande importância para a indústria vitivinícola e constitui um defeito que aparece por contaminação dos vinhos. Esta contaminação é normalmente atribuída à rolha de cortiça e o 2,4,6-tricloroanisol (TCA) é o composto mais frequentemente associado a este “off-flavour”.

Neste trabalho, um painel de consumidores efectuou ensaios triangulares de resposta obrigatória, com vista à determinação dos Limiares de Detecção Olfactivos (LDO) e Limiares de Detecção Gustativos (LDG) do TCA em água, soluções hidroalcoólicas (11,5 e 18% etanol) e vinho de mesa branco e tinto.

Um ensaio de comparação por pares foi utilizado pelo painel para avaliar o Limiar de rejeição Olfactivo (LRO) em vinhos brancos e vinhos tintos aos quais foi adicionado TCA.

Os resultados obtidos mostram que o LDO e LDG em água correspondem respectivamente a 0,2 e 0,3 ng/L, em soluções hidroalcoólicas a 11,5 e 18% o LDO foi de 4 e 10ng/L respectivamente. Nos vinhos tintos o LDO e LDG foi de 0,9 e 1,7 ng/L e nos vinhos brancos foi respectivamente 1,5 e 1,0. O LRO obtido para o vinho branco foi de 10,4ng/L e para o vinho tinto 16,0 ng/L. Os resultados obtidos indicam que, embora este grupo de consumidores tenha detectado a presença de TCA em baixas concentrações nas diferentes amostras testadas, não rejeitaram as amostras de vinho que apresentavam estes teores.

RÉSUMÉ

2,4,6-Tricloroanisol: évaluation par un group de consommateurs

Le «goût de bouchon» est un problème important dans l’industrie vinicole et est provoqué par la contamination des vins. Cette contamination est habituellement attribuée aux bouchons de liège et le 2,4,6-trichloroanisole (TCA) est l’un des composés la plupart du temps associés à ce goût.

Dans ce travail, un panel de consommateurs a effectué des essais triangulaires de choisi «forcé» afin de mesurer les seuils de détection d’odeur (SDO) et les seuils de détection de goût (SDG) de TCA en eau, solutions hydroalcooliques (éthanol de 11.5% et de 18%) et vins blancs et rouges.

Un épreuve de préférence par paire a été également exécuté par le panneau afin de mesurer le seuil de rejet d’odeur (SRO) en vin blanc et rouge pointu avec TCA.

Les résultats obtenues pour les SDO et les SDG pour TCA dans l’eau étaient 0.2 et 0.3 ng/L, respectivement. Dans les solutions hydroalcooliques avec de l’éthanol de 11.5% et de 18% les SDO étaient 4 et 10 ng/L respectivement. En vin rouge les SDO et les SDG étaient 0.9 et 1.7 ng/L et en vin blanc était 1.5 et 1.0 ng/L respectivement. SRO pour le blanc était 10.4 ng/L et pour les vins rouges 16.0 ng/L.

Ces résultats suggèrent que bien que ce groupe de consommateurs ait détecté des concentrations très basses de TCA en vins, ils n’aient pas rejeté le vin à ces valeurs basses de concentration.

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Bertrand A., 1998. Les differentes formes de «goût de bouchon» dans le vin. In: XXIII Congrés Mondial de la Vigne et du Vin- Vol. II Lisboa, 585-591.

Bertrand A. , Barrios M.L., 1994. Contamination de bouchons par les produits de palettes de stockage des bouteilles. Rev. Fran. OEnologie, 149: Nov/Dec.

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sorptive extraction and gas chromatography-mass spectrometry. Talanta, (in press) doi: 10.1016/ j.talanta.2006.09.020.

Casey J., 1999. T´ain’t necessarily so. History and research shed light on cork’s role in musty/ mouldy taints of bottled wine. Wine Industry Journal, 14 (6), 49-56.

Cantagrel R., Vidal J. P., 1990. Research on compounds responsible for cork taint in cognacs. In: 6th

International Flavor Conference, Flavors and Off-flavors Elsevier Science pp. 139-157.

Chatonnet P., Guimberteau G., Dubourdieu D. Boindron, J.N., 1994. Nature et origine des odeurs de « moisi » dans les vaves. Influence sur la contamination des vins. J. Int. Sci. Vigne Vin, 28, 131-151.

Chatonnet P., Labadie M-D, 1995. Contamination des locaux vinicoles et altérations des vins-contrôle de qualité de l’atmosphère des chais. Rev. Fr. Oenol., 74, 19-21.

Chatonnet P., Bonnet S., Bouton S., Labadie M-D. (2004) Identification and responsability of 2,4,6-tribromoanisole in musty, corked odors in wine. J. Agri. Food Chem., 52, 1255-1262. Curtis R.F., Land D.G., Griffiths N.M., Gee M., Robinson D., Peel J.L., 1974. Chloroanisoles a cause of musty taint in chicken and their microbiological formation from chlorophénols. J. Sci. Food Agric., 25, 811-828.

Delwiche J., 2004. The impact of perceptual interactions on perceived flavour. Food Quality and Preference, 15, 137-146.

Ezquerro O., Tena M.T., 2005. Determination of odour-causing volatile organic compounds in cork stoppers by multiple headspace solid-phase microextraction. J. Chromatogr. A, 1068, 201-208.

Fischer C., Fischer U., 1997. Analysis of cork taint in wine and cork material at olfactory sub threshold levels by solid phase micro extraction. J. Agri. Food Chem., 45, 1995-1997. Griffiths N.M., 1974. Sensory properties of chloroanisols. Chemical Senses Flavour, 1, 187-195.

Insa S., Salvadó V., Anticó E., 2006. Assays for the simultaneous determination of chloroanisols and chlorophenols from contaminated cork samples. J. Chromatogr. A, 1122, 215-221. ISO, 2004. Standard 4120: Sensory Analysis- Methodology- Triangular test

ISO, 1992. Standard 5492: Sensory Analysis- Vocabulary

ISO, 2005. Standard 5495: Sensory Analysis- Methodology- Paired comparison test

Lorenzo C., Zalacain A., Alonso G.L., Salina M.R., 2006. Non destructive method to determine halophenols and haloanisoles in cork stoppers by headspace sorptive extraction. J. Chromatogr. A, 1114, 250-254.

Montiel A., Rigal S., Welté B., 1999. Study of the origin of musty taste in the drinking water supply. Water Science and Technology, 40 (6), 171-177.

Moore E., Pravda M., Guilbault G., 2003. Development of a biosensor for the quantitative detection of 2,4,6-TCA using screen printed electrodes. Anal. Chim. Acta, 484, 15-24. Ochiai N., Yamashita S., Daishma S., Heiden A., Hoffman A., 2001. Determination of trace amounts of off-flavor compounds in drinking water by stir bar sorptive extraction and thermal desorption GC-MS. Analyst, 126 (10), 1652-1657.

Pereira C.S., Marques J.J., San Romão M.V., 2000. Cork taint in wine: scientific knowledge and public perception- a critical review. Crit. Rev. Microbiol., 26 (3), 147-162.

Prescott J., Norris L., Kunst M., Kim S., 2005. Estimating a «consumer rejection threshold» for cork taint in white wine. Food Quality and Preference, 16 (4), 345-349.

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Rui M., Mestres M., Busto O., Guash J., 2006. Determination of total chloroanisols in different kind of cork stoppers. Anal. Chim. Acta 563, 310-314.

Sanvicens N., Sanchez-Baeza F., Marco M.-P., 2003. Immunochemical determination of 2,4,6-trichloroanisole as the responsible agent for the musty odour in foods. 1. Molecular modelling studies for antibody production. J. Agri. Food Chem., 51(14), 3924-3931.

Soleas G., Yan J. Seaver T., Goldberg D., 2002. Method for the gas chromatographic assay with selective detection of trichloro compounds in corks and wines applied to elucidate the potential cause of cork taint. J. Agri. Food Chem., 50 (5), 1032-1039.

Suprenant A., Butzke C.E., 1997. Implication of odor threshold variations on sensory quality control of cork stoppers. Am. Journal Enol. Viticul., 48 (2) 269.

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