Article 2022 Detection Wine Alterations Sensory An

Medicon Agriculture & Environmental Sciences
Volume 2 Issue 1 January 2022

Research Article
Detection of Wine Alterations by Sensory Analysis: Overview of Results obtained from

Interlaboratory Tests
Caterina Mazzoni*, Anne Tirard and Abdelkader Boubetra

BIPEA (Bureau Interprofessionnel des Etudes Analytiques), Scientific and Technical Department, 189 rue d’Aubervilliers, Paris, France
*Corresponding Author: Caterina Mazzoni, BIPEA, Scientific and Technical Department, 189 rue d’Aubervilliers, Paris, France.
Received: December 16, 2021; Published: December 28, 2021
Abstract
Throughout history wine has been appreciated thanks to its distinctive sensory characteristics. Wine quality control is crucial
for wine producers, which need to identify any alterations throughout all the winemaking process. Among the techniques used to
determine the quality of wines, the most important is sensory evaluation by trained experts, as it is directly related to the organ-
oleptic characteristics of wines. However, wine is a complex matrix and several factors can affect assessors’ perception. The same
defect can be perceived at different intensities according to experience, training and cultural origins of the panel. This could be
problematic for winemakers who need to have an objective analysis. Participation in interlaboratory studies is an interesting tool
for a sensory analysis laboratory that needs to demonstrate that its results are the same as those obtained by other laboratories
or bodies. Moreover, participation in interlaboratory tests can provide precious information about the performance of assessors.
The purpose of this paper is to critically summarize results obtained from interlaboratory tests for the identification of a main
defect in wines which have been artificially contaminated.
Keywords: sensory analysis; wine defects; wine quality control; interlaboratory test; tasting panel; olfactory alterations; taste
and tactile alterations
Introduction
A wine can be defined as altered when an undesirable compound is present at a concentration above the detection limit. The latter
can be very variable depending on the substance, whose concentration can be measured in grams, milligrams, micrograms or even
nanograms per litre.
Molecules responsible for wine alteration may have different origins [1]. Some defects are directly linked to grapes and abnormal-
ities resulting from the maturity of the grapes and/or fungal diseases. Other ones, related to the techniques used, pre-fermentation
operations or alcoholic fermentation, can be attributed to the main products of yeast and bacterial metabolism or be directly associ-
ated with bacterial metabolism.
Negative attributes of wines can be classified in visual, olfactory, taste and tactile alterations.
The main visual alterations are hazy appearance, browning and pinking effect on white wine, and, for red wines, lack of colour and
premature brick-red colour. Causes of these defects are various: hazy appearance is due to the presence of yeasts and bacteria, proteins
or tannins, browning and pinking effect are caused respectively by the oxidation of polyphenols or phenolic acids and the presence
of polyphenols and an excess of sulphites. Lack of colour of red wines is related to lack of pigments and an excess of sulphites and the
cause of premature brick-red colouris an insufficient tannin-anthocyanin combination.
The best-known taste and tactile alterations, acidity, bitterness and astringency are considered defects only when they impact ex-
Citation: Caterina Mazzoni., et al. “Detection of Wine Alterations by Sensory Analysis: Overview of Results obtained from Interlaboratory Tests”.
Medicon Agriculture & Environmental Sciences 2.1 (2022): 04-13.
Detection of Wine Alterations by Sensory Analysis: Overview of Results obtained from Interlaboratory Tests
05
cessively the wine structure. Acidity is due to the presence of an excessive amount of tartaric or malic acids which give to wines a taste
of unripe grape and lemon. Wine tannins or grape tannins are the main elements responsible for the bitter defect (raw chicory, pure
cocoa, green tea, quinine taste) and the astringent tactile alteration as feeling of dryness and roughness in the mouth [2]. Other taste
alterations can be due to the presence of acetyltetrahydropyridine (odour reminiscent of mouse and acetamide) or excess of ethyl
hexanoate or decanoate (taste of soap).
Among olfactory alterations, the attributes vegetable, mouldy, acetic, reduced, oxidised, animal and lactic are the most frequent
terms mentioned by tasters.
The main molecules responsible for vegetable attributes are methoxypyrazines, which give the wine herbaceous notes (green
pepper, ivy) and 1-hexanol, which is found in the wine as a result of the mechanical crushing of the skins and which also gives distinct
notes of cut grass [3].
The mouldy defects (also known as corked taste) are considered among the most harmful because they cannot be eliminated. This
detrimental taste effect is generally perceived as a musty earthy aroma (musty-dusty, musty and/or damp cellar) that can mask the
natural nuances of the wine and irreversibly affect its quality [4]. Although various compounds have been identified in relation to this
spoilage [5, 6], most authors in the literature agree that haloanisoles, particularly chloroanisoles, are the main compounds responsi-
ble for this problem [7]. These molecules come from the transformation by moulds of less-odorous halophenols into highly-odorous
haloanisoles by methylation in a humid atmosphere and in a confined environment.
Geosmin, 2-isopropyl-3-methoxypyrazine and 2-methyl-isoborneol, responsible for the wet-earth, earthy-mould and mushroom
odours and tastes (earthy defect), originate from agro-viticultural factors, such as berries with fragile skins and undesirable mould
attacks.
The 1-octen-3-one gives wines a fresh mushroom smell. Although difficult to eliminate, its presence can be ephemeral.
The acetic attribute refers principally to the presence of acetic acid or ethyl acetate. Acetic acid, which produces a pungent, acrid
smell in the nose and a bitter taste in the mouth, is one of the best-known defects. This molecule can develop through the presence
of acid rot on the grapes or contamination by indigenous yeasts. It can also be produced during alcoholic fermentation, by yeasts or
lactic bacteria or, in the refining phase, by acetic bacteria. Ethyl acetate, which is responsible for the odours of glue, nail polish and/or
solvent, is mainly attributable to the indigenous yeast micro flora present on the grapes. It is produced by yeasts and acetic bacteria
during alcoholic fermentation or by acetic bacteria during the ageing and storage phase of the wine.
The reduced defect is due to the presence of volatile sulphonated compounds, responsible for rotten-egg, gas, garlic and cabbage
odours, which are mainly generated by yeasts during alcoholic fermentation. These molecules include ethanethiol, mercaptans and
hydrogen sulphide.
Acetaldehyde gives the wine an odour of stale apple and/or rancio, whichare descriptors of the oxidised attribute. This aldehyde
is the result of the metabolism of yeasts or bacteria and the oxidising process of the wine in contact with oxygen. If in red wines its
presence in small quantities is positive, as it favours the stabilisation of the colour and the polymerisation of phenolic compounds, in
excess or in white wines it can be considered a defect.
Diacetyl is responsible forlactic, buttery, butyric odours in wines (the lactic attribute). This molecule is produced by lactic bacteria
during malolactic fermentation. Similar fermentative aromas are also given by other compounds such as ethyl lactate, acetoin, butane-
diol and pentanedione.
The animal attribute is used to describe phenolic, leather, stable, horse-sweat or foxy odours in wine. These defects have different
origins. The o-aminoacetophenone is responsible for the foxy odour. The biochemical mechanisms that cause its formation have not
06
yet been fully elucidated. During the bottle-ageing phase, some dry white wines show signs of premature ageing, such as the change of
colour to orange tones and the loss of the fruity aromas typical of young wines. Phenolic, stable, horse-sweat odour can be associated
with the presence of 4-ethylphenol and 4-ethylguaiacol [8]. The4-ethylguaiacol is an aromatic phenol compound found in red wines
contaminated by Brettanomyces spp. It is not a particularly unpleasant substance in itself, as it is smoky and spicy, but its presence is
often associated with that of 4-ethylphenol. The latter mainly affects the fruit note and the wine is more astringent when tasted. 4-eth-
ylguaiacol is derived from phenolic acids, constituents of the grape, which are transformed into 4-ethylphenol by the double action of
decarboxylation and reduction.
Lastly, wines can be affected by other olfactory alterations due to specific compounds such as benzaldehyde (bitter-almond, bug,
specific unpleasant odour), 4-vinylphenol and 4-vinylguaiacol (pharmaceutical, medicinal odour), cresols (camphorated and iodinat-
ed odours), biogenic amines (mousy taste, rotten meat and putrefaction), dimethyl disulphide (cabbage odour) 1,6-trimethyl-1,2-di-
hydronaphthalene (hydrocarbon odour).
Any wine alteration must be identified as soon as possible throughout all the winemaking process. Nowadays, sophisticated chemi-
cal analytical methods are used to characterize wine and to investigate any presence of unwanted compounds. To identify organoleptic
defects, chemical analysis of wine is generally accompanied by sensory evaluation by trained experts. In the last few years, the number
of laboratories who wish to incorporate a sensory analysis process into their quality system is increasing. However, authorized accred-
itation bodies only accredit objective sensory tests which are properly documented and validated. In this framework, participation
in interlaboratory tests can provide precious information about the performance of assessors. Thanks to this tool, a sensory analysis
laboratory has the possibility to demonstrate that its results are the same as those obtained by other panels. Nevertheless, wine is a
complex alcoholic beverage and several factors can affect assessors’ perception. The same defect can be perceived at different intensi-
ties according to the panel experience, training and cultural origins.
This work describes results obtained in interlaboratory tests on wines artificially altered with a specific compound. Over three
years, 14 different wines were submitted to laboratories. Each wine proposed was altered with a molecule that corresponds to a main
olfactory, taste or tactile alteration. The perception of the defects mouldy-earthy, acetic, reduced, oxidized, animal, acid, bitter, and
astringency was tested.
These tests were not implemented for sensory analyses of wines, but their principal objective was to test laboratories in finding a
main defect artificially added to matrices.
Materials and Methods
Aninterlaboratory test entails the analysis by different laboratories of the same analytical parameters on identical samples. The
setting up of these tests can be schematized by 3 main steps: preparation of homogenous samples, analyses by the laboratories and
the statistical treatment of the data.
Sample production and shipment
The most crucial aspect for the implementation of an interlaboratory testprogramme is the production of homogeneous and stable
samples. For this study, all samples of wine proposed were spiked to obtain a main defect. By basing these interlaboratory tests on the
notion of a flagrant defect, the spiking concentrations were above the detection limits of the molecules. The wines’ characteristics, and
their spiking levels by matrix and by attribute are summarized in Table 1. After spiking, matrices were homogenized in a dedicated
glass vessel with a floating cover. Sufficient contact time for mixing (defect + wine) was guaranteed (between 1 and 3 days, according
to the spiking molecule). Samples were packaged in glass vials with no headspace and stored in a thermostatic chamber at 12-20°C.
Homogeneity and stability check of the batches were performed according to the requirements of ANNEX B of the ISO 13528
standard [9]. For both studies, chemical analyses to confirm the same concentration of the spiked molecule in tested samples were
07
performed according to the Compendium of the OIV (International Organization of Vine and Wine) [10].
Analyses and statistical treatments
Prepared samples were sent to laboratories, without any indication about the spiking molecules (blind test). Given the nature of
the product, participants must organize the sensory sessions as soon as possible after the reception of the samples. Laboratories were
invited to follow the analysis method prescribed by OIV [11]. The tasting panel must be composed of a minimum of 10 assessors in
order to be taken into account in the statistical treatment. Reply forms indicate the main visual, olfactory, taste and tactile alterations:
- Visual alterations:
Hazy appearance
Browning
Pinking effect (white wine)
Lack of colour (red wine)
Premature brick-red colour (red wine)
- Olfactory alterations:
Vegetable
Mouldy-earthy
Acetic
Reduced
Oxidized
Animal
Lactic
Other notes (to specify).
- Tactile and taste alterations:
Acid
Bitter
Astringency.
Assessors were invited to evaluate the alterations according to an intensity scale from zero (if the attribute is not found as a wine
adulteration) to 5. A value higher than zero is an indication of the defect identified. If the wine presents more than one defect, attri-
butes must be evaluated individually.
The intensity of the negative attributes predominantly perceived must also be indicated, as well as acceptance or refusal of the tested
wine. An Excel file was sent to panels for individual data. Median, inter-quartile range, robust standard deviation, relative coefficient
of variation, higher and lower confidence intervals were calculated for each tasting panel. Medians of intensity of each defect were
represented graphically. As an example, the graph of results of the panel of a laboratory participant to the test on red wine spiked with
4-ethylphenol is shown in Figure 1.
The data of each tasting panel were collected and treated statistically: for a given wine and for each defect, the median of the in-
tensity level of a perceived defect was estimated from data indicated by panels. The results were presented graphically in the final
statistical report for each attribute. An example of graphical representation of medians of the intensities returned by each panel for a
specific alteration is shown in Figure 2. The median of medians of the intensity of perceived defect of laboratories for which the panel
was composed by at least 10 assessors is indicated as a line in these graphs.
08
Figure 1: Graphical representation of results obtained by the tastingpanel of a laboratory par-

ticipating in the test on red wine spiked with 4-ethylphenol. The x-axis lists the different defects
that could be found in wine. The y-axis represents the medians of the intensity of perception of
each defect detected by tasters. Olfactory alterations are indicated in green, tactile and taste ones
in red. The tasting panel of this laboratory detected the main defect caused by the presence of
4-ethylphenol (animal olfactory alteration), with an intensity of 5 (high level).
Figure 2: Graphical representation of medians obtained by laboratories on the animal defect

perception for a red wine spiked with 4-ethylphenol.
All laboratories participating to this test are represented in the x-axis using a confidential code.
The y-axis represents the medians of the intensity of perception of the animal olfactory alter-
ation detected by tasting panels of each laboratory. The green line indicates the median of the
medians of laboratories which panel consists of at least 10 assessors (selected laboratories).
Results and Discussions
The number of participating laboratories, mainly from Europe and America, varies from 15 to 31, depending on the trial. An over-
view of the results of the tests is summarized in Table 1. Results are satisfactory: the main laboratories found the defect linked to the
presence of the spiking molecule in almost all the proposed samples. Even if wines with a neutral sensory profile were chosen for these
tests, adding some molecules can alter the sensory equilibrium and highlight also defects which were not the target. Radar charts rep-
resenting the intensity of each perceived defect on each proposed wine are shown in Figure 3. In these graphs, dotted lines represent
the medians of intensity of defects perceived by laboratory and red continuous lines indicate the medians of these medians.
Four different samples were proposed for detection of mouldy-earthy alteration in red wines. Two wines were spiked with trichlo-
roanisole (TCA) and geosmin was added to the other two samples.
09
Trichloroanisole spiking concentrations were 38 ng/L for the first trial and 29 ng/L for the second one. Mouldy-earthy olfactory
alteration was indicated by 61% of participants for the first tests and 83% for the second one. The medians of the intensity of perceived
alteration of selected laboratories were 3 and 4 respectively. It can be noticed that results of the second test were more satisfactory, the
same defect was detected by a larger population of laboratories and the median obtained was higher even if the spike concentration
was lower. The olfactory identification of trichloroanisole can be difficult due to the influence of the matrix, the difference in sensitiza-
tion of the panel, the training of the panel and finally the rapid saturation of sensory receptors.
Spiking concentrations of geosmin were 702 ng/L and 451 ng/L respectively. 88% out of laboratories participating in the first test
detected the mouldy-earthy alteration. All of the laboratories participating to the second one detected this defect. The median of the
intensity of perceived this defect was 4 for the two tests, despite the difference in spiking concentration.
Two different tests were organized for the acetic olfactory alteration: white wine samples were spiked with ethyl acetate at 160
mg/L for the first test and 226 mg/L for the second one. Acetic defect was not indicated as a glaring defect by the laboratories partic-
ipating to the first test, even if the amount added to the wine normally allows detection of this defect. Only 20% out of participating
laboratories found this alteration. The predominant negative attributes were acidic for 30% of the laboratories and bitter for 20%
of participants (taste alterations). In the second test, 60% of the laboratories detected the acetic defect due to the presence of ethyl
acetate in the wine. The higher concentration of this molecule in wine allowed more consistent results compared to the first test, the
medians of the intensity of perceived alteration of these two tests were 1 and 3 respectively. Moreover, a wine with different character-
istics was chosen for the second test and this may have played a role in the degree of perception of acetic defect.
Laboratories Intensity of Laboratories

Alteration mole- WineCharacteristics1 and Spiking Con- Number of
identifying the perceived refusing wine
cule / Defect test centration participants
main defect (%) main defect2 (%)
Red wine (Merlot, Langued-
oc Roussillon) 38 ng/L 31 61% 3 90
Trichloro anisole T1 ME
Mouldy-earthy Red wine (Syrah,

LanguedocRoussillon) 29 ng/L 15 83% 4 100
T2 ME
Red wine (Merlot, Langued-
ocRoussillon) 702 ng/L 15 83% 4 100
Geosmin T3 ME
Red wine (Shiraz, Syrah,
Mouldy-earthy Grenache, Carignan, Cotes
451 ng/L 18 100% 4 100
du Rhone)
T4 ME
White wine (Chardonnay,
LanguedocRoussillon) 160 mg/L 15 20%3 1 25
Ethyl acetate T1 Acetic
Acetic White wine (Sauvignon,
Grenache, Vaucluse) 226 mg/L 18 60% 3 100
T2 Acetic
10
Laboratories Intensity of Laboratories

Alteration mole- WineCharacteristics1 and Spiking Con- Number of
identifying the perceived refusing wine
cule / Defect test centration participants
main defect (%) main defect2 (%)
White wine (Sauvignon,
Grenache, Cotes du Rhone) 59 ng/L 15 45%4 2 93
Ethanethiol T1 Reduced
Reduced Red wine (Syrah,
LanguedocRoussillon) 81 μg/L 18 60% 3 94
T2 Reduced
White wine (Colom-
Acetaldehyde bard,Ugniblanc, Listan,
135.6 mg/L 18 89% 4 100
Oxidized Gascogne)
T1 Oxidized
Red wine (Merlot,
4-Ethylphenol
LanguedocRoussillon) 441 μg/L 15 100% 4 87
Animal
T1 Animal
White wine (Sauvignon,
LanguedocRoussillon) 2.2 g/L 31 16%5 4 97
Tartaric acid T1 Acid
Acid White wine (Sauvignon,
LanguedocRoussillon) 1.1 g/L 15 50% 3 60
T2 Acid
White wine (Chardonnay,
Quinine Sulphate
LanguedocRoussillon) 28.3 mg/L 15 63% 3 50
Bitter
T1 Bitter
Red wine (Merlot,
Grape tannins
LanguedocRoussillon) 1087 mg/L 15 56% 3 71
Astringency
T1 Astringency
1. Grape variety and origin
2. Median of selected panels
3. 30% of laboratories detected the “Acid” defect, median: 2
4. 33% of laboratories detected the “oxidized” defect, median: 2
5. 68% of laboratories detected the “Mouldy-earthy” defect, median: 4
Table 1: Summary of results obtained in interlaboratory tests for identification of wine defects.
For the detection of reduced defect, a white and a red wine were spiked with ethanethiol at a concentration of 58 ng/L and 81 mg/L
respectively. 44% of the laboratories detected the reduced defect in white wine, even if the median of the intensity of this perceived
alteration was low (2). In this same sample, 33% of laboratories indicated the oxidized defect. 60% of the laboratories detected the
reduced defect in the red wine (3 was the median of the intensity). The higher concentration and the different wine characteristics
likely contributed to the improved results of this second test.
Concerning the oxidized defect, white wine samples were spiked with acetaldehyde at 135.6 mg/L; 89% of the laboratories detected
the presence of this alteration in wine. The median of the intensity of perceived defect of selected laboratories was 4.
For the detection of the animal defect, a test on red wine samples spiked with 4-ethylphenol at 441 mg/L was organized. 100% of
the laboratories detected this olfactory alteration. The median of the intensity of perceived defect of selected laboratories was 4.
11
Two different tests were proposed for the acid taste alteration: white wine samples were spiked with tartaric acid at 2.2 g/L for the
first test and 1.1 g/L for the second one. Only 16% of laboratories participating to the first test found the acid defect as the major one.
Two different tests were proposed for the acid taste alteration: white wine samples were spiked with tartaric acid at 2.2 g/L for the
first test and 1.1 g/L for the second one. Only 16% of laboratories participating to the first test found the acid defect as the major one.
The median of the intensity of perceived taste alterations of selected laboratories was 4. The analysis of laboratories’ results showed
also a mouldy-earthy olfactory alteration, with a median of the intensity equal to 4. This negative attribute, detected by 68% of the
participants, mainly derives from the matrix. Concerning the second test, 50% of the laboratories detected the acid alteration.
Quinine sulphate was added to white wine samples at a concentration of 28.3 mg/L to highlight the bitter defect. 63% of the labo-
ratories detected this alteration, with a median of the intensity of the perceived defect of 3.
Finally, red wine samples were spiked with grape tannins: 56% of the laboratories detected the astringency defect due to the pres-
ence of excess tannins in wine. The median of the intensity of the perceived defect of selected laboratories was 3.
Almost all wines were refused by the majority of panels, except the first white wine spiked with ethyl acetate, which was refused
only by 25% of participants. However, it is important to remember that wine is a very complex matrix and a defect perception may be
influenced by the characteristics of the spiked product.
12
Figure 3: Radar charts of panel results for identification of alterations in wines. Studied wines
and spiking molecules are indicated at the top of each graph. The red continuous line indicates
the median of the medians of intensity of defects perceived by laboratories (dotted lines).
Conclusion
Results obtained in overall tests highlight that some alterations are well-known and easier identified by panels (i.e., mouldy-earthy
and animal). In general, laboratories better detect the artificially added defect if the molecule responsible for the alteration has al-
ready been proposed in previous tests. Data concerning the intensity of the main perceived defect consolidate this observation as low
dispersions of panellists’ answers is noticed when laboratories are faced with an alteration for the second time. These results show
that interlaboratory tests support laboratories in their process of continuous improvement and can be useful as sensory training to
improve tasters’ sensibility, providing precious information about the performance of assessors.
13
In conclusion, sensory analysis is an excellent tool for wine quality control, as the product is analysed in its entirety. As any scientific
tool, this discipline requires a lot of rigour to guarantee reliable and quality results. Authorized accreditation bodies only accredit
objective sensory tests which are properly documented and validated: participation in interlaboratory tests is an interesting tool for
laboratories for satisfying the conditions required by the ISO/IEC 17025 standard [12] and gaining the trust of accreditation bodies
and customers.
Acknowledgements
BIPEA acknowledges all laboratories participating in these PTS.
References
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Laks PE, New York (1992): 859-880.
3. Allen MS and Lacey MJ. “Methoxypyrazines of grapes and wines”. Chemistry of Wine Flavor, ACS Publications Washington DC
(1998): 31-38.
4. Silva Pereira C., et al. “Cork taint in wine: scientific knowledge and public perception. A critical review”. Crit Rev Microbiol 26.3
(2000): 147-162.
5. Amon JM., et al. “Compounds responsible for cork taint”. Aust NZ Wine Ind J 4 (1989): 62-69.
6. Peña-Neira A., et al. “Presence of cork-taint responsible compounds in wines and their cork stoppers”. Eur Food Res Technol 211
(2000): 252-256.
7. Chatonnet P., et al. “Identification and responsibility of 2,4,6-tribromoanisole in musty, corked odors in wine”. J. Agric. Food Chem
52.5 (2004): 1255-1262.
8. Tempere S., et al. “The olfactory masking effect of ethylphenols: Characterization and elucidation of its origin”. Food Quality and
Preference 50 (2016):135-144.
9. ISO/IEC 13528:2015 - Statistical methods for use in proficiency testing by interlaboratory comparisons.
10. International Organisation for Vine and Wine - OIV Compendium of International Methods of Wine and Must Analysis 2 (2017).
11. OIV Review document on sensory analysis of wine (2016).
12. ISO/IEC 17025:2017 - General requirements for the competence of testing and calibration laboratories.
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Medicon Agriculture & Environmental Sciences

Volume 2 Issue 1 January 2022

Detection of Wine Alterations by Sensory Analysis: Overview of Results obtained from

Caterina Mazzoni*, Anne Tirard and Abdelkader Boubetra

Materials and Methods

Sample production and shipment

Analyses and statistical treatments

Figure 1: Graphical representation of results obtained by the tastingpanel of a laboratory par-

Figure 2: Graphical representation of medians obtained by laboratories on the animal defect

Results and Discussions

Laboratories Intensity of Laboratories

Mouldy-earthy Red wine (Syrah,

Laboratories Intensity of Laboratories

BIPEA acknowledges all laboratories participating in these PTS.

1. Navarre C and Langlade F. L’œnologie, Lavoisier, Paris (2010).

Volume 2 Issue 1 January 2022

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