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Food Control 18 (2007) 398–403
www.elsevier.com/locate/foodcont
Aroma proWle of wines from Albillo and Muscat grape
varieties at diVerent stages of ripening
E. Sánchez Palomo a, M.C. Díaz-Maroto a,b,¤, M.A. González Viñas a,
A. Soriano-Pérez a, M.S. Pérez-Coello a
a
Área de Tecnología de los Alimentos, Facultad de Ciencias Químicas, Universidad de Castilla-La Mancha,
Campus Universitario 10, 13071 Ciudad Real, Spain
b
IRICA (Instituto Regional de Investigación CientíWca Aplicada), Universidad de Castilla-La Mancha,
Campus Universitario 10, 13071 Ciudad Real, Spain
Received 11 July 2005; received in revised form 23 November 2005; accepted 26 November 2005
Abstract
Volatile composition of musts and wines from Muscat “a petit grains” and Albillo grape cultivars harvested at diVerent states of ripening,
was evaluated. Among the volatile compounds analysed by GC/FID/MS, wines obtained from less ripe grapes displayed higher ester and
fatty acid concentrations, but less terpene compounds and benzene derivatives, than wines from grapes with a high degree of maturity. Maturity also greatly inXuenced wine aroma. In all cases, wines from grapes with higher sugar content were more fruity and less vegetal and Xoral.
© 2005 Elsevier Ltd. All rights reserved.
Keywords: Aroma; Wine; Grape; Ripening; OAV
1. Introduction
Wine aroma is formed by hundreds of volatile compounds of diVerent chemical natures and origins, found at a
wide range of concentrations.
Compounds arising from grape metabolism (terpenes,
norisoprenoids, benzene compounds and C6 alcohols) vary
as a function not only of the variety but also of certain cultural and climate-related factors (Bureau, Razungles, &
Baumes, 2000; Jackson & Lombard, 1993; Zoecklein, Wolf,
Marcy, & Jasinski, 1998). These compounds can appear
either in their free form, playing a key role in the quality
and the peculiar aroma of wines, especially in aromatic
grape varieties such as Muscat, or bound to sugar mole-
*
Corresponding author. Address: Área de Tecnología de los Alimentos,
Facultad de Ciencias Químicas, Universidad de Castilla-La Mancha,
Campus Universitario 10, 13071 Ciudad Real, Spain. Tel.: +34 926 295300;
fax: +34 926 295318.
E-mail address: MariaConsuelo.Diaz@uclm.es (M.C. Díaz-Maroto).
0956-7135/$ - see front matter © 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.foodcont.2005.11.006
cules, being odourless (Günata, Bayonove, Baumes, &
Cordonnier, 1985; Williams, Sefton, & Wilson, 1989).
In neutral grape varieties, other compounds formed during yeast fermentation or released from conjugated forms
by chemical or enzyme hydrolysis may play a more important role in the overall aroma of the wine (Cabaroglu, Canbas, Lepoutre, & Günata, 2002; Sefton, Francis, &
Williams, 1993). In this respect, the processing techniques
or the type of yeast strain used may prompt some modiWcation of the Wnal aroma, although the contribution of the
grape variety predominates (Antonelli, Castellari, Zambonelli, & Carnacini, 1999; García Romero, Pérez Coello,
Cabezudo, Sánchez-Muñoz, & Martín-Alvarez, 1999).
One of the factors most inXuencing the aroma characteristic of a given variety is the stage of ripening of the grape.
Both free and glycosylated forms of varietal compounds
are accumulated in the grape during ripening (Bayonove,
1993). Terpene content may decrease once optimal sugar
levels are attained, although this may be inXuenced by temperature and water availability during ripening (RibereauGayon, Glories, Maujean, & Dubourdieu, 2000).
E.S. Palomo et al. / Food Control 18 (2007) 398–403
The time of harvest is traditionally governed by must
sugar content, or determined by reference to certain indices linking sugar content with acidity (Ribereau-Gayon
et al., 2000). However, these indices are not always
matched by the aromatic maturity of the grape (Girard,
Fukumoto, Mazza, Delaquis, & Ewert, 2002; Schneider,
Razungles, Charrier, & Baumes, 2002). Advanced grape
maturity and greater exposure to the sun favour the accumulation of varietal compound in the berry (Schneider
et al., 2002). Lower canopy densities may produce an
increase in glycosidically-bound compounds in the berry
(Jackson & Lombard, 1993; Zoecklein et al., 1998).
Late-harvested Garnacha grapes yielded wines with less
-ionone and cis-3-hexen-1-ol and more -damascenone
and geraniol than those early-harvested (Sabon, Revel,
Kotseridis, & Bertrand, 2002).
However, not all volatile compounds aVect the overall
wine aroma. The olfactory perception threshold for each
compound varies considerably; the olfactory impact of a
compound will thus depend on whether it is present at
concentrations above this threshold. Over recent years,
sniYng techniques, calculation of olfactory thresholds for
a wide range of compounds, and the use of OAVs (odour
activity values) have enabled the identiWcation of numerous odorants in wines from several grape varieties (Guth,
1997; Lopez, Ortín, Pérez-Trujillo, Cacho, & Ferreira,
2003; Schneider, Razungles, Augier, & Baumes, 2001).
Muscat “a petit grains” is an aromatic variety containing a fairly typical amount of terpene compounds, although
less than Muscat of Alexandria (Bureau et al., 2000; Castro
Vázquez, Pérez Coello, & Cabezudo, 2002). Since Albillo is
a neutral variety and has a low terpene content, it has been
traditionally used as table grape. However, recent studies
have demonstrated that wines made from Albillo grapes
contain interesting Xavour notes (Jurado, Pinilla, Ballesteros, Pérez-Coello, & Cabezudo, 2001).
The purpose of this study was to determine the eVect of
the grape ripening degree on the aroma of wines made
under the same fermentation conditions, using one aromatic variety (Muscat “a petit grains”) and one neutral
variety (Albillo), both grown in a sunny and warm climate.
2. Materials and methods
2.1. Samples
Grapes from Vitis vinifera varieties Muscat “a petit
grains” and Albillo cultivated in the La Mancha region
(Spain) were harvested at diVerent stage of ripening in two
vintages. Laboratory fermentations using 3 L vessels were
carried out in duplicate, and inoculated with Saccharomyces cerevisiae race cerevisiae yeasts (CECT no. 10835).
2.2. Isolation of volatile compounds
Varietal compounds were extracted from musts and
wines using the method developed by Günata et al. (1985).
399
Two hundred millilitres of must or wine were fractionated
on preconditioned styrene-divinylbenzene cartridges (Bond
Elut, Varians, 1 g of phase), using 4-nonanol as internal
standard, with subsequent elution with 50 mL of pentane–
dichloromethane (2:1). Extracts were concentrated on a
Vigreux column to a Wnal volume of 200 L.
Fermentation compounds were isolated by continuous
liquid–liquid extraction with pentane–dichloromethane
(60:40). 4-Nonanol was used as internal standard. The
extracts obtained were concentrated on a Vigreux column
and injected into a GC column.
2.3. Gas chromatography conditions
A Hewlett–Packard model 4890 gas chromatograph
equipped with a Xame ionisation detector (280 °C) was used
with a BP-21 capillary column (50 m £ 0.32 mm i.d.; 0.32 m
Wlm thickness). Injector temperature was 250 °C and
oven temperature was set at 70 °C (5 min), then raised at
1 °C/min to 95 °C(10 min), and then raised at 2 °C/min to
190 °C (40 min). Carrier gas was He (0.7 mL/min). Injection
volume was 1 L in splitless mode (0.6 min).
IdentiWcation was made by comparison of GC retention
times with those of authentic standards from Sigma–Aldrich, and by CG–MS (Hewlett–Packard G 1800 B GCD
System). For quantiWcation purposes, calibration curves
were used when standards were available, otherwise semiquantitative analysis was performed assuming a response
factor equal to one.
3. Results and discussion
Table 1 shows results for °Brix, pH, and total acidity
of musts obtained from Albillo and Muscat “a petit
grains” varieties harvested in both 2001 and 2002,
together with some of the most widely used maturity indices (Coombe, Dundon, & Short, 1980; Ellis, Van Rooyen,
& Du Plessis, 1985). With reference to the results for
°Brix, it should be pointed out that the 2001 harvest was
delayed, and grapes of both varieties were riper than
grapes from the 2002 vintage. As was to be expected, total
acidity was lower for the 2001 harvested grapes, although
acidity results for Muscat “a petit grains” were still
higher than expected. Attending the maturity indices,
although the most widely used is the °Brix/volatile acidity
ratio, a value of 3.1 being considered optimal for grapepicking, indices involving pH are considered better
predictors of harvest quality.
The optimal value for °Brix £ pH2 lies between 200 and
270, while for °Brix £ pH, the optimum is between 85 and
95 (Boulton, Singleton, Bisson, & Kunkee, 1996). There was
no correlation between these indices, in our results for Muscat “a petit grains” grapes, the 2001 vintage had a acceptable maturity index according to the °Brix/volatile acidity
ratio, but not using the others two indices. In Albillo grapes
the °Brix £ pH index was adequate for the 2001 vintage but
not the other two indices.
400
E.S. Palomo et al. / Food Control 18 (2007) 398–403
Table 1
°Brix, pH, total acidity and maturity indices of musts obtained from Muscat “a petit grains” and Albillo varieties from the vintages 2001 and 2002
°Brix
pH
Total acidity (g (H2T)/L)
°Brix/total acidity (g (H2T)/L)
°Brix £ pH2
°Brix £ pH
Muscat “a petit grains” 2001
Muscat “a petit grains” 2002
Albillo 2001
Albillo 2002
26.5
3.3
8.3
3.2
288.6
87.5
21.6
3.2
8.6
2.5
221.2
69.1
25.1
3.5
4.2
6.0
307.5
87.9
21.6
3.3
5.7
3.8
235.2
71.3
Table 2
Volatile compound concentration (g/L) of musts obtained from Muscat “a petit grains” and Albillo varieties from the vintages 2001 and 2002
Compounds
Muscat “a petit grains” 2001
Muscat “a petit grains” 2002
Albillo 2001
Albillo 2002
Mean
Mean
RDS (%)
Mean
RDS (%)
Mean
55.1
218.5
6.3
59.9
391.1
7.4
5.9
11.9
1.5
1.5
40.0
113.9
18.0
28.3
274.2
6.3
5.1
3.6
11.5
4.9
19.3
140.9
15.9
17.0
284.3
RDS (%)
2-Hexenal
1-Hexanol
(E)-3-Hexen-1-ol
(Z)-3-Hexen-1-ol
(E)-2-Hexen-1-ol
37.3
63.9
34.1
3.5
102.7
6.8
8.3
4.9
5.7
5.6
Total C6 compounds
241.5
Benzaldehyde
Benzyl alcohol
2-Phenylethanol
116.4
118.0
Total benzenic compounds
234.4
Geraniol
Linalool
Hotrienol
-Terpineol
Citronellol
Nerol
Geranic acid
165.6
197.5
82.6
36.9
8.7
3.4
4.1
11.9
103.0
4.6
Total monoterpenes
585.6
730.9
9.8
10.3
6.8
142.8
102.0
514.2
11.9
9.7
11.4
251.6
110.3
103.0
13.7
9.5
6.4
104.1
100.2
545.2
Tr
60.9
51.1
112.0
8.2
11.2
4.3
9.7
9.8
9.7
1.0
RDS (%)
4.1
2.4
1.8
0.8
1.8
477.4
7.8
6.1
7.9
133.1
54.9
5.1
11.0
11.4
188.0
13.4
2.5
13.4
2.5
Tr: traces.
In conclusion the utility of these indices is limited and
they do not oVer information about the quality of wines
obtained. The aroma is one of the main factors related to
the quality of white wines and compounds responsible for
wine aroma should be taken in account in the evaluation of
the optimal stage of grape ripening.
Results for quantiWcation of the varietal compounds in
Albillo and Muscat musts for both harvests are shown in
Table 2. Muscat musts from the 2002 vintage, when harvested
grapes were less ripe, displayed higher C6 alcohol concentrations than those harvested in 2001. By contrast, concentrations of terpene compounds (monoterpenes and oxygenated
terpenes) were lower in 2002. Similar Wndings are reported by
other authors for a number of grape varieties (Bureau et al.,
2000; Sabon et al., 2002; Schneider et al., 2002).
In the Albillo variety, however, little terpene compounds
were detected, and C6 alcohol levels were very similar for
both harvests, although slightly higher for 2001. The opposite was true of benzene compounds. The results for a given
harvest may be strongly inXuenced by weather factors (temperature, rainfall) during ripening (Marais, Van Wik, &
Rapp, 1992), and results for volatile composition varied
between harvests for the same grape variety, independently
of sugar content (Dieguez, Lois, Gómez, & de la Peña,
2003).
During the fermentation process varietal compounds
can suVer some changes, for instance 1-hexanol was greater
in wines than in musts and (E)-2-hexen-1-ol and 2-hexenal
were not detected in wines, probably due to transformations by yeast metabolism.
On the other hand in Muscat a petit grains wines some
monoterpenes, such as linalool, hotrienol and citronellol,
were higher than in the must, but others decreased: geraniol
and nerol.
Table 3 shows the varietal compound concentrations
of wines from Muscat “a petit grains” and Albillo for the
two vintages. Regarding the total amounts, Muscat “a
petit grains” wines from 2002 contained higher C6 alcohol than wines from 2001 vintage. However Albillo wines
displayed similar C6 alcohol content in both vintages.
More terpene compounds were found in Muscat “a petit
grains” wines; concentration were lower in 2002, as they
were for musts. Benzene compounds were lower in 2002 for
Muscat wine.
With regard to fermentation compounds (Table 4), production of fatty acid esters and acetates was lower in 2002,
E.S. Palomo et al. / Food Control 18 (2007) 398–403
401
Table 3
Varietal compounds concentration (g/L) of wines obtained from Muscat “a petit grains” and Albillo varieties from the vintages 2001 and 2002
Compounds
Muscat “a petit
grains” 2001
Muscat “a petit
grains” 2002
Mean
RDS (%)
Mean
1-Hexanol
(E)-3-hexen-1-ol
(Z)-3-hexen-1-ol
267.8
46.5
18.5
3.2
2.6
11.9
547.6
38.6
36.1
Total C6 compounds
332.8
Geraniol
Linalool
Hotrienol
-Terpineol
Citronellol
Nerol
Geranic acid
20.6
273.5
138.2
34.0
27.8
Tr
171.5
Total monoterpenes
665.6
Benzaldehyde
Benzyl alcohol
Tr
594.6
Total benzenic compounds
594.6
Albillo
2001
RDS (%)
7.2
5.3
0.9
622.3
7.0
2.9
5.7
3.5
8.7
Mean
RDS (%)
Mean
RDS (%)
481.6
87.6
44.9
6.0
7.4
2.5
607.8
52.2
10.8
2.2
4.4
13.5
614.1
61.6
147.7
93.9
39.2
100.7
Tr
84.4
5.9
Albillo
2002
670.8
3.1
7.0
4.2
9.5
1.4
1.5
3.2
1.5
Tr
226.1
6.9
15.6
527.5
6.6
327.4
12.9
3.2
3.6
0.1
334.0
Tr
219.6
–
9.4
219.6
226.1
Tr: traces.
Table 4
Volatile compounds from fermentation (mg/L) of wines obtained from Muscat “a petit grains” and Albillo varieties from the vintages 2001 and 2002
Compounds
Acetaldehyde
Methanol
1-Propanol
Isobutanol
3-Methyl-1-butanol
2-Methyl-1-butanol
3-(Methylthio)-1-propanol
2-Phenylethanol
Total alcohols
Muscat “a petit
grains” 2001
Muscat “a petit
grains” 2002
Albillo
2001
Mean
Mean
Mean
45.2
61.2
14.2
14.9
87.0
17.9
0.5
20.1
67.9
5.3
0.05
0.2
0.9
1.2
1.1
1.0
0.3
10.1
Total esters
88.0
Total acids
0.1
4.5
1.6
0.6
0.7
1.4
3.0
7.7
261.0
Ethyl acetate
Isoamyl acetate
Hexyl acetate
Phenylethyl acetate
Ethyl lactate
Ethyl hexanoate
Ethyl octanoate
Ethyl decanoate + Isovaleric acid
Diethyl succinate
Ethyl 4-hydroxybutyrate
Isobutyric acid
Butyric acid
Hexanoic acid
Octanoic acid
Decanoic acid
RDS (%)
0.8
0.9
4.9
6.2
2.7
15.5
44.5
21.5
24.0
28.9
167.2
42.5
0.9
15.8
RDS (%)
8.6
4.3
4.1
4.9
2.0
4.3
3.5
7.2
345.3
1.9
12.6
8.7
9.2
0.3
6.3
2.3
4.3
8.6
10.5
24.9
1.7
0.01
0.01
0.6
0.5
0.3
2.2
0.06
7.6
1.5
0.7
2.0
3.0
0.7
7.9
but fermentation alcohols were slightly higher in this case.
Given that fermentation conditions and the yeast strain
used were the same, diVerences observed in both varieties
may be attributed to the diVerent sugar content and must
composition between vintages.
RDS (%)
Mean
RDS (%)
0.5
1.2
1.6
2.9
10.1
2.8
8.0
4.7
19.8
27.0
10.0
17.6
123.7
45.4
1.4
31.0
2.5
10.1
15.9
4.4
2.0
10.0
3.3
1.6
209.6
9.5
0.2
9.9
17.3
2.1
4.6
3.1
22.6
5.4
24.4
37.88
2.0
11.7
9.2
10.4
3.4
14.3
37.7
14.2
15.2
86.2
21.4
0.4
20.2
Albillo
2002
46.0
2.9
0.03
0.1
0.4
1.2
1.0
0.9
0.2
13.1
275.9
1.7
2.3
1.5
2.7
4.9
8.8
2.6
5.6
8.7
8.4
65.83
5.1
17.8
5.2
6.1
0.6
1.2
0.4
4.4
5.5
1.7
13.2
20.9
3.7
0.03
0.2
1.1
0.7
0.8
2.3
0.1
6.8
1.8
0.3
11.9
10.7
4.9
8.8
6.1
3.4
6.2
1.0
36.63
3.0
2.7
3.0
2.4
7.9
1.7
0.6
2.1
3.4
1.0
11.0
8.7
2.0
2.5
6.1
8.8
In order to assess the inXuence of the compounds studied on overall wine aroma, odor activity values (OAV)
were calculated by dividing the concentration of each
compound by its perception threshold. Of all the compounds analysed, only those displaying OAVs greater
402
E.S. Palomo et al. / Food Control 18 (2007) 398–403
Table 5
Odour activity values (OAVs) of volatile compounds with more inXuence in the aroma of wines obtained from Muscat “a petit grains” and Albillo varieties harvested in 2001 and 2002
Compounds
Sensory descriptor
Odour threshold
(g/L)
Muscat “a petit
grains” 2001
Muscat “a petit
grains” 2002
Albillo
2001
Albillo
2002
Linalool
Geraniol
Hotrienol
2-Phenylethanol
Acetaldehyde
3-methyl-1-butanol
3-(Methylthio)-1-propanol
Ethyl acetate
Isoamyl acetate
Ethyl hexanoate
Ethyl octanoate
Flowery
Citric
Hyacinth
Roses, sweet
Pungent, ripe apple
Burnt, alcoholic
Cooked vegetables
Fruity, solvent
Banana
Fruity, green apple, banana
Fruity, banana, pineapple,
peach, sweet
Sweet, grass
Rancid
Cheese
Grass acid
15a
30a
110b
10 000a
500a
30 000a
500a
7500a
30a
5a
2a
18.18
0.67
1.25
2.02
90.50
2.90
1.07
9.05
177.37
239.23
547.50
9.85
2.05
0.85
1.58
89.09
5.57
1.80
3.33
58.19
91.02
151.25
2.02
28.68
2.87
1.05
6.14
94.36
236.43
527.33
3.10
39.63
4.12
2.77
2.79
121.93
132.97
392.54
2.01
20.00
1.63
12.4
5.00
41.92
0.65
6.08
1.75
16.57
1.46
11.00
4.75
37.43
0.71
6.81
Ethyl decanoate
Isovaleric acid
Hexanoic acid
Octanoic acid
a
b
c
200c
33.4c
3000a
500c
Guth (1997).
Etiévant (1991).
Ferreira et al. (2000).
than 1 were deemed to contribute to wine aroma (Guth,
1997).
Table 5 shows the OAVs for the compounds that have
values greater than 1, together with sensory descriptors and
the perception threshold taken from the literature.
Muscat “a petit grains” contained a group of compounds with Xoral or citric odours, i.e. terpenes (linalool,
hotrienol, and geraniol). Other terpenes identiWed,
including citronellol and -terpineol, were present at concentrations below, although occasionally close to the
odour threshold. These compounds give to Muscat wines
their characteristic aroma, and there may be some synergic eVect involving all the monoterpenes that gives rise to
the deWning “moscatel” aroma (Ribereau-Gayon et al.,
2000).
In wines made from grapes harvested in 2002, hotrienol
concentrations were below its odour threshold, while geraniol concentrations were above it. The terpene displaying
the highest OAV value was linalool; similar Wndings have
been reported for other aromatic varieties including Albariño and Gewürztraminer (Falqué, Fernandez, & Dubourdieu, 2001; Ong & Acree, 1999).
C6 alcohols were present at concentrations below their
odour thresholds in all cases. Fermentation alcohols with
major sensory impact were 2-phenylethanol, which displayed a characteristic rose aroma and 3-methyl-1-butanol.
Medium-chain fatty acid esters and acetates tend to
present fruity aromas and may play a major sensory role,
especially in neutral grape varieties containing negligible
amounts of terpenes (Cabaroglu et al., 2002; Lopez et al.,
2003). Ethyl octanoate and hexanoate displayed high OAV
values in both wines and for both vintages.
Some fatty acids were present at levels over the perception threshold in both grape varieties. These compounds
displayed fatty aromas, cheesy or rancid, that were not perceived in the overall wine aroma, perhaps because they
were overwhelmed by other more intense aromas. The same
was true for the “boiled-vegetable” aroma of 3-methylthiopropanol.
The tasting panel scored wines made from Muscat “a
petit grains” as having a intense, Xoral, typically “Muscat”
aroma, and a moderate fresh and fruity odour. Wines from
Albillo grapes had citric and fruity aromas (melon, green
apple, peach), with Xoral notes. In all cases, wines from the
2002 harvest scored lower than those of the 2001 harvest in
terms of aroma intensity.
Acknowledgements
The authors thank to the Ministerio de Educación y
Ciencia (project AGL2004-07205) and to Mercadona S. A.
for the Wnancial support, and to M. Dolores Cabezudo for
her scientiWc assistance. Eva Sánchez-Palomo would like to
thank the Ministerio de Educación, Cultura y Deporte for
the award of a grant.
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