Food Research International 156 (2022) 111178

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Food Research International

journal homepage: www.elsevier.com/locate/foodres

Combined effects of the vessel type and bottle closure during Chilean
Sauvignon Blanc wine storage over its volatile profile
Cristina Ubeda a, b, Álvaro Peña-Neira c, Mariona Gil i Cortiella d, *
a
Departamento de Nutrición y Bromatología, Toxicología y Medicina Legal, Facultad de Farmacia, Universidad de Sevilla, C/Profesor García González 2, 41012 Sevilla,
Spain
b
Instituto de Ciencias Biomédicas, Facultad de Ciencias de la Salud, Universidad Autónoma de Chile, Chile
c
Facultad de Ciencias Agronómicas. Universidad de Chile, Avenida Santa Rosa 11315, 8820808 Santiago, Chile
d
Instituto de Ciencias Químicas Aplicadas, Facultad de Ingeniería, Universidad Autónoma de Chile, El Llano Subercaseaux 2801, San Miguel, Chile

A R T I C L E I N F O A B S T R A C T

Keywords: A Sauvignon Blanc wine was subjected to a maturation period of six months by using four different types of
Volatile compounds vessels in triplicate: cylindrical stainless steel tanks, oval-shaped polyethylene tanks, cubic-shaped polyethylene
Sauvignon Blanc tanks, and clay jars. After maturation in the different vessels, wines were bottled using three different closures
Stainless steel
(natural cork, synthetic cork, and screwcaps). The volatile compound profiles of the wine samples were recorded
Clay
by SPME-GC–MS throughout vessel maturation as well as after the bottle storage period. In general terms, wines
Polyethylene
Natural cork stored in stainless steel tanks showed the highest contents of volatile compounds when compared with the other
Synthetic cork tested vessels. Moreover, wines from bottles capped with screwcaps showed the highest contents of most of the
Screwcap volatile compounds when compared with the other closures. Moreover, an interaction between the vessel and the
Wine maturation closure was observed: when screwcaps were used during bottle aging, the resulting wines were very similar to
those matured in stainless steel vessels. These results suggest that the use of screwcaps hides the differences
originating from wine composition during maturation in vessels other than stainless steel.

1. Introduction behavior against atmospheric oxygen since wine exposure to oxygen

Traditionally, wines have been produced and stored mainly in
stainless steel vats and oak barrels. However, in the last decade, a set of
new types of vessels made with different materials (such as concrete,
clay, granite, polyethylene, etc.) and with different shapes (ovoid,
spherical, tulip, etc.) have been incorporated in wineries, modifying
their inner skyline. Good examples for this trend are the high number of
brands that could be found in the market corresponding to wines elab­
orated in clay jars or amphoras, utilizing such ancient vessels to elabo­
rate distinctive wines (Cabrita et al., 2018; Díaz, Laurie, Molina,
Bücking, & Fischer, 2013; Martins et al., 2018). Several implications of
the use of alternative vessels to conventional vessels (stainless steel vats
and oak barrels) were reported regarding their effects on the elemental
composition, volatile compound profiles, and sensory attributes (Cabrita
et al., 2018; Díaz et al., 2013; Gil i Cortiella, Ubeda, Covarrubias, Laurie,
& Peña-Neira, 2021; Gil i Cortiella, Úbeda, Covarrubias, & Peña-Neira,
2020; Martins et al., 2018).
One of the main features of winemaking vessels is related to their
during elaboration has a great influence on the final characteristics of
the resulting wines (del Alamo-Sanza, Laurie, & Nevares, 2015; del
Alamo-Sanza & Nevares, 2018; Nevares & del Alamo-Sanza, 2021). In
that sense, materials such as concrete, clay, or polyethylene allow oxy­
gen to permeate through the vessel walls, likely what happens with oak
barrels (Nevares & del Alamo-Sanza, 2021). In contrast, such materials
do not release sensory active compounds, as occurs with oak barrels
(providing volatile compounds and tannins to wines). Thus, winemakers
like to use these types of materials for wine maturation since they allow
a slow oxygenation of wines (contrary to what happens with stainless
steel vats) without altering the sensory profile and typicality of wines (as
occurs by using oak barrels).
In addition to the vessel employed during winemaking for wine
storage and maturation, the closure employed at bottling also impacts
the oxygenation rate of wines. The traditional closure for wine bottles is
natural cork, which allows slow oxygenation of wines during bottle
aging. In addition, natural cork is also related to the sorption and/or
desorption of chemicals between closure and wine (Furtado et al.,

* Corresponding author.
E-mail address: mariona.gil@uautonoma.cl (M. Gil i Cortiella).

https://doi.org/10.1016/j.foodres.2022.111178
Received 30 November 2021; Received in revised form 18 March 2022; Accepted 20 March 2022
Available online 23 March 2022
0963-9969/© 2022 Elsevier Ltd. All rights reserved.
C. Ubeda et al.
Fig. 1. Box plots for each volatile compound family throughout aging in the different types of vessels tested. The line inside the box shows the mean.
2021). In addition to natural cork, two other types of closures have been
widely employed for wine preservation: synthetic cork and screwcaps.
Both closures prevent the contamination of wines with 2,4,6-trichloroa­
nisole (TCA), a volatile compound that confers a moldy off-flavor
(usually known as cork taint) to the wines and comes from fungal
contamination of the natural cork material during its production (Peña-
Neira, Simón, Cadahía, & Suarez, 2000; Pereira, Marques, & San, 2000;
Sefton & Simpson, 2005). Even though synthetic corks avoid the risk of
cork taint, they show a high permeability to oxygen, and the mass
transfer of chemical compounds between closure and wine could take
place during post-bottling maturation of wines (Furtado et al., 2021).
Screwcaps are metallic closures (usually made of aluminum) that screw
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Food Research International 156 (2022) 111178
onto threads in the neck of the bottle (Furtado et al., 2021). The oxygen
permeability of screw caps depends mainly on the inner liner, a thin
layer made of polymeric materials that helps to maintain compression
and prevent gas exchange (He, Zhou, Peck, Soles, & Qian, 2013).
Given that both the vessel and the closure employed impact the ox­
ygen exposure of wines (Waterhouse et al., 2016), it would be expected
that the resulting wines would show different characteristics. Indeed, it
has been reported that oxygen exposure during wine production
severely impacts the volatile compound profiles of the resulting wines
(Coetzee & Du Toit, 2015; Coetzee, Lisjak, Nicolau, Kilmartin, & du Toit,
2013; Ugliano, 2013), which in turn is closely related to the sensory
aromatic perception of wines (Goniak & Noble, 1987; González Álvarez,
C. Ubeda et al.
Fig. 2. Averaged Odor Activity Values (OAV) of individual volatile compounds from the wines during the six months period of vessel storage. The odor thresholds
employed to calculate the OAV are shown in Table 3. The dotted line indicates the OAV = 1.
González-Barreiro, Cancho-Grande, & Simal-Gándara, 2011; Revi,
Badeka, Kontakos, & Kontominas, 2014; Verzera et al., 2008).
Although the effect of vessel and the effect of bottle closure has been
previously studied, in our knowledge, it is the first time that both factors
are studied together. Thus, the present study contains the volatile pro­
files of Sauvignon Blanc wines stored in different types of vessels in
triplicate (by using three stainless steel tanks, three polyethylene oval-
shaped tanks, three polyethylene tanks with cubic shape, and three
clay jars) for six months, followed by six more months of bottle aging
using three different closures (natural cork, synthetic cork, and screw­
cap). Such data help to better understand the impact of the vessel on
wine volatile compound contents as well as the interaction between the
vessel employed during winemaking and the bottle closure employed
during bottle maturation of wines.
2. Methods and materials
2.1. Trial conditions
The wine used for this trial corresponded to a monovarietal Sau­
vignon Blanc wine made with grapes from the Curicó Valley in Chile
[35◦ 00′ 41.288′ ’ S; 71◦ 14′ 51.999′ ’ W] harvested during the 2017
vintage. The wine was elaborated in the winery Miguel Torres Chile
located in the same valley following a conventional white winemaking
procedure using a stainless-steel tank with a 50.000 L capacity equipped
with a cooling system, where the wine was maintained from alcoholic
fermentation to the beginning of the trial (approximately two months
later). The general parameters of the raw wine determined according to
the official methods (International Organisation of Vine and Wine,
2016) were 12% vol. ethanol content, a titratable acidity of 5.7 g/L
(expressed as tartaric acid equivalents), and a pH of 3.0. In addition, the
raw wine had a color intensity of approximately 0.10 (expressed as the
sum of absorbances at 420 nm, 520 nm, and 620 nm measured using a
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Food Research International 156 (2022) 111178
cuvette with a 10 mm light path) and a phenolic index of 6.6 (expressed
as the 280 nm absorbance measured using a quartz cuvette with a
10 mm light path, corresponding to the I280 reported elsewhere
(Ribéreau-Gayon, Glories, Maujean, & Dubourdieu, 2006b)). Such wine
(corresponding to the t0 sample) was used to fill the different types of
vessels (without having carried out any stabilization treatment) in
triplicate: [CYL] 150 L cylindrical stainless steel tanks (Navarro y Cia.
Ltda., Santiago, Chile); [OVO] 980 L oval-shaped polyethylene tanks
(Apollo FLEXTANK, Partner Ltd., Santiago, Chile); [CUB] 1000 L cubic
polyethylene tanks (FLEXTANK, Partner Ltd., Santiago, Chile); and
[JAR] 225 L clay jars (Value Juices Ltd., Santiago, Chile). Thus, a total of
12 vessels were used for this trial. The wine was maintained in the
vessels for six months of storage, and a sample of wine was taken from
each vessel once every 1.5 months to assess the evolution of volatile
profiles of wines throughout vessel storage. After six months of matu­
ration in the vessels, the wine from each vessel was bottled in green glass
bottles (750 mL) using three different caps: [SCR]: screw cap (with a
liner allowing low rates of oxygen intake, Empack, Santiago, Chile),
[SINT]: synthetic cork (HST, Santiago, Chile), and [NAT]: natural cork
(Corpack ACI, Santiago, Chile). The bottles were stored in an under­
ground dark cellar (18 ± 1 ◦ C) in a horizontal position for six months,
after which the volatile composition of wines was determined, to assess
the evolution of volatile profiles of wines throughout bottle storage.
2.2. Analysis of volatile compounds of wine samples by SPME-GC–MS
The analysis of the volatile composition of the samples was carried
out following the method described in Ubeda et al. (2017). Samples from
the vessel storage trial were processed the day after they were taken, and
the samples after bottle aging were immediately processed after opening
the bottle. For the extraction of volatile compounds, the solid phase
microextraction (SPME) technique was used as follows: 7.5 mL of sam­
ple was placed into a 20 mL glass vial containing 1.5 g of sodium
C. Ubeda et al. Food Research International 156 (2022) 111178

Table 1
Quantification (μg/L) of the main chemical families of volatile compounds during wine storage in the different types of vessels. The norisoprenoids family were
expressed as relative areas. Different capital letters in a column indicate significant differences (p < 0.05, Duncan’s post hoc test) among storage times for the same
volatile compound and the same type of vessel. Different lowercase letters in a row indicate significant differences (p < 0.05, Duncan’s post hoc test) among types of
vessels for the volatile compound and the same storage time. The p-interaction value between vessel and storage time factors is indicated in addition to the VOC noun as
follows: * indicates p < 0.05; ** indicates p < 0.01; *** indicates p < 0.001.
VOC TIME CYL OVO CUB JAR

Total esters t0 305862 ± 55695B 305862 ± 55695B 305862 ± 55695B 305862 ± 55695B
t1 204971 ± 26312 A 197734 ± 7836 A 189259 ± 15456 A 197762 ± 8215 A
t2 236972 ± 22810 AB 206462 ± 22422 A 202662 ± 12421 A 229356 ± 14623 A
t3 252553 ± 33339 AB ab 261776 ± 11158 AB b 196768 ± 5051 A a 227445 ± 34385 A ab
t4 231684 ± 19222 AB 226965 ± 16913 A 265511 ± 11718B 243967 ± 5703 A
Total ethyl esters t0 24370 ± 4332B 24370 ± 4332C 24370 ± 4332C 24370 ± 4332B
t1 10896 ± 1346 A 9076 ± 408 A 9605 ± 774 A 9448 ± 511 A
t2 12295 ± 2017 A b 8582 ± 1548 A a 9546 ± 783 A ab 10353 ± 143 A ab
t3 15642 ± 4096 A ab 16090 ± 1271B b 10577 ± 2218 A a 13574 ± 3711 A ab
t4 15500 ± 3983 A 14019 ± 1599B 16834 ± 427B 15326 ± 995 A
Total acetate esters t0 28467 ± 3408B 28467 ± 3408C 28467 ± 3408B 28467 ± 3408B
t1 14920 ± 2593 A 13759 ± 757 A 13757 ± 956 A 13326 ± 1009 A
t2 16233 ± 2299 A b 12156 ± 1004 A ab 13516 ± 847 A a 13733 ± 1253 A ab
t3 17655 ± 3658 A ab 18164 ± 1048B b 13029 ± 1108 A a 15507 ± 2884 A ab
t4 15570 ± 2550 A 14414 ± 1269 A 12002 ± 10475 A 14928 ± 208 A
Total alcohols * t0 220113 ± 23864C 220113 ± 23864C 220113 ± 23864B 220113 ± 23864C
t1 137222 ± 14381 A 134589 ± 7412 A 129225 ± 6174 A 136447 ± 3242 A
t2 151309 ± 15940 AB 138824 ± 5729 A 135020 ± 1513 A 143714 ± 4154 A
t3 200096 ± 14623 BC b 210497 ± 6439C b 143698 ± 12953 A a 171496 ± 33500 AB a
t4 188454 ± 35647 BC 186704 ± 5594B 205571 ± 4191B 202084 ± 5267 BCE
Total acids * t0 18662 ± 682 18662 ± 682C 18662 ± 682C 18662 ± 682B
t1 14155 ± 854b 12389 ± 769 A a 12002 ± 651 A a 12312 ± 165 A a
t2 16795 ± 1177b 13015 ± 1745 A a 12820 ± 98 A a 13473 ± 1120 A a
t3 16027 ± 2125b 15670 ± 663B b 11995 ± 422 A a 12876 ± 1140 A a
t4 17251 ± 3418 13052 ± 961 A 14740 ± 2146B 12989 ± 1289 A
Total terpenes t0 120.5 ± 5.2 120.5 ± 5.2B 120.5 ± 5.2B 120.5 ± 5.2
t1 101.4 ± 5.2b 92.4 ± 4 A ab 88.8 ± 5.6 A a 95.9 ± 3.9 ab
t2 103.3 ± 13.6 91.7 ± 7.7 A 84.1 ± 10.0 A 95.2 ± 4.7
t3 110.6 ± 11.0 ab 123.5 ± 6.1B b 76.6 ± 11.7 A a 93.3 ± 24.4 ab
t4 115.7 ± 34.5 110.9 ± 8.2B 119.7 ± 12.7B 110.5 ± 3.6
Total norisoprenoids t0 72.4 ± 2.4B 72.4 ± 2.4C 72.4 ± 2.4B 72.4 ± 2.4B
t1 48.2 ± 6.1 A 44.1 ± 8.6 A 44.4 ± 6.4 A 50.1 ± 9.0 A
t2 57.3 ± 3.0 AB 53.1 ± 10.1 AB 49.7 ± 7.1 A 58.3 ± 11.8 AB
t3 45.8 ± 11.4 A a 65.2 ± 6 BC b 36.9 ± 5.9 A a 43.3 ± 8 A a
t4 61.7 ± 14.2 AB 56.5 ± 8.9 ABC 56.6 ± 18.9 AB 54.6 ± 8.9 AB
Total thiols t0 237.7 ± 22.2B 237.7 ± 22.2C 237.7 ± 22.2C 237.7 ± 22.2C
t1 140.2 ± 15.4 A 134.1 ± 3.6 A 124.6 ± 6 A 130.2 ± 11.4 A
t2 153.2 ± 9.0 A 136.5 ± 19.6 A 122.8 ± 3.2 A 135.6 ± 9.8 A
t3 189.6 ± 32.5 AB 197.8 ± 6.8B 134.5 ± 25.5 A 151.8 ± 31.7 A
t4 205.3 ± 47.5 AB 190.5 ± 6.3B 192.6 ± 13.4B 194.7 ± 19.3B
TOTAL VOLATILE COMPOUNDS t0 545067 ± 80006B 545067 ± 80006C 545067 ± 80006B 545067 ± 80006B
t1 356638 ± 41506 A 344983 ± 15884 A 330744 ± 22243 A 346797 ± 11434 A
t2 405389 ± 39901 A 358582 ± 24299 A 350758 ± 13108 A 386832 ± 18964 A
t3 469021 ± 50112 AB b 488330 ± 9597 BCE b 352709 ± 17852 A a 412104 ± 68933 A ab
t4 437772 ± 57844 AB 427079 ± 16674 AB 486191 ± 18099B 459400 ± 6783 AB

chloride (analytical grade, Merck) and 10 μL of 4-methyl-2-pentanol
(0.75 mg/L), which was added as an internal standard. Samples were
incubated at 45 ◦ C with agitation (500 rpm) for 20 min to saturate the
headspace with volatiles. After this time, the SPME fiber (2 cm 50/30 µm
Carboxen/DVB/PDMS SPME fiber; Supelco, Bellefonte, PA, USA) was
exposed to the vial headspace for 40 min. Once finished, the compounds
from the fiber were desorbed into the GC injector port of a 7890B Agilent
GC system (Agilent Technologies, Palo Alto, CA, USA) and injected using
the splitless mode (3 min) and a transfer line temperature of 280 ◦ C. The
gas chromatograph was equipped with a DB Wax capillary column
(60 m × 0.25 mm, and 0.25 μm film thickness; J&W Scientific, Folsom,
CA, USA), and the helium flow rate was set at 1 mL/min as the carrier
gas. The oven program temperature was set at 35 ◦ C for 1 min, increased
to 130 ◦ C at 12 ◦ C/min and held for 1 min, then to 160 ◦ C at 1 ◦ C/min,
and subsequently raised to 220 ◦ C at 10 ◦ C/min with holding for 10 min.
The detection was performed by an Agilent 5977 mass spectrometer,
with electron ionization mass spectra in the scan mode recorded at 70 eV
in the range of 35 to 300 u. MS ChemStation software (Agilent Tech­
nologies) was employed for the analysis of chromatograms. The iden­
tification of compounds was performed by comparing spectra with the
NIST database library (version 2.0) and linear retention index (LRI) of
authentic standards, calculated by retention times of n-alkanes (C6-C30)
under identical conditions for each analysis program. When standards
were not available, the compounds were tentatively identified using
NIST and the literature. Regarding quantitation, calibration curves of
reference standards were determined to express the results by the means
of the concentration. The compounds from every chemical group were
calibrated in specific ranges of concentration based on the usual con­
centrations present in wine. Hence, esters were calibrated from 1 to
15000 µg/L; alcohols from 1 to 50000 µg/L extended to 300 mg/L for
isoamyl alcohol; terpenes from 0.25 to 50 µg/L extended to 200 50 µg/L
in the case of nerol oxide employing limonene; acids from 10 to 10000
µg/L; norisoprenoids were expressed in relative areas. Again, in the
cases in which no standards were available, the data were expressed in
relative area dividing the peak area of the target ion (major ion) by the
peak area of the target ion of the internal standard. These cases are
indicated in the foot table of Tables 1S and 2S..

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Table 2
Quantification (μg/L) of the main chemical families of volatile compounds after six months of bottle storage. The norisoprenoids family were expressed as relative
areas. Different capital letters in a column indicate significant differences (p < 0.05, Duncan’s post hoc test) among cap types for the same volatile compound and the
same type of vessel. Different lowercase letters in a row indicate significant differences (p < 0.05, Duncan’s post hoc test) among types of vessels for the same volatile
compound and the same cap type. The p-interaction value between vessel and cap factors is indicated in addition to the VOC noun as follows: * indicates p < 0.05; **
indicates p < 0.01; *** indicates p < 0.001.
VOC CAP CYL OVO CUB JAR

Ethyl esters (excluding Ethyl Acetate) NAT 14824 ± 181b 12111 ± 699 AB a 11742 ± 118 A a 11229 ± 670 A a
SINT 14335 ± 593b 10560 ± 1105 A a 11559 ± 1335 A a 10942 ± 2000 A a
SCR 16227 ± 1686 16879 ± 489B 15682 ± 1532B 15256 ± 1070B
Acetate esters (excluding Ethyl Acetate) NAT 4535 ± 524b 2412 ± 545 ab 2570 ± 132 a 2655 ± 955 ab
SINT 4078 ± 493b 1708 ± 341 a 2724 ± 1357 ab 2442 ± 153 a
SCR 3918 ± 449 5748 ± 3145 3692 ± 2285 3255 ± 2092
Other esters NAT 576 ± 104b 338 ± 162 a 250 ± 127 A a 316 ± 160 a
SINT 620 ± 65b 330 ± 160 a 368 ± 135 AB a 316 ± 118 a
SCR 881 ± 237b 619 ± 81 ab 568 ± 2B a 536 ± 166 a
Total esters (excluding Ethyl Acetate) NAT 19935 ± 653b 14861 ± 1374 A a 14561 ± 362 a 14199 ± 1593 A a
SINT 19033 ± 1053b 12598 ± 1511 A a 14651 ± 2805 a 13700 ± 2159 A a
SCR 21027 ± 1949 23247 ± 3693B 19941 ± 3592 19047 ± 2971B
Total C6 alcohols NAT 1586 ± 185b 1357 ± 18 A a 1336 ± 37 a 1425 ± 106 a
SINT 1597 ± 56b 1519 ± 126 AB ab 1364 ± 233 ab 1244 ± 202 a
SCR 1627 ± 191 1882 ± 385B 1572 ± 283 1618 ± 331
Total alcohols NAT 147391 ± 13634b 125276 ± 1735 A a 125819 ± 5325 A a 124558 ± 1484 a
SINT 150694 ± 14650b 123854 ± 8413 A a 132763 ± 4368 AB ab 128137 ± 8899 a
SCR 150855 ± 14373 160432 ± 19631B 152855 ± 17761B 140837 ± 15085
Total C6 compounds ** NAT 5868 ± 1190 AB b 5474 ± 261b 3718 ± 382 A a 5071 ± 263b
SINT 6483 ± 887B 5796 ± 126 5934 ± 634B 5420 ± 473
SCR 4402 ± 610 A a 5166 ± 1124 ab 6115 ± 930B b 4865 ± 592 ab
Total acids * NAT 10452 ± 1676b 7002 ± 1036 a 6073 ± 845 A a 7926 ± 958 a
SINT 11359 ± 2758b 7359 ± 765 a 8952 ± 1108B ab 7789 ± 1185 a
SCR 9706 ± 100b 8740 ± 913 ab 9766 ± 1724B b 6817 ± 686 a
Total terpenes NAT 225 ± 25b 186 ± 14 AB a 182 ± 8 a 180 ± 9 A a
SINT 210 ± 10 178 ± 35 A 177 ± 31 162 ± 25 A
SCR 238 ± 32 237 ± 29B 217 ± 23 240 ± 12B
Total Norisoprenoids NAT 135 ± 12B b 116.7 ± 10.2 A a 105.3 ± 2.5B a 100.6 ± 10.2 A a
SINT 96.9 ± 5.7 A b 76.1 ± 9.9 A a 68.9 ± 10.1C a 67.8 ± 11.4 A a
SCR 167.8 ± 17.4C 178.6 ± 40.2B 180.2 ± 7.2 A 166.2 ± 30.6B
Total thiols NAT 120 ± 28b 107 ± 10b 51 ± 6 A a 121 ± 28b
SINT 120 ± 28 99 ± 12 104 ± 21B 100 ± 20
SCR 161 ± 31 113 ± 31 146 ± 35B 162 ± 47
TOTAL VOLATILE COMPOUNDS * NAT 391812 ± 26811b 333514 ± 4687 A a 329193 ± 10990 A a 337725 ± 20436 a
SINT 413728 ± 47904b 319083 ± 14652 A a 350792 ± 24506 A ab 343882 ± 39384 a
SCR 410369 ± 21564 452042 ± 48229B 418448 ± 43018B 401557 ± 42606

2.3. Odor Activity values
The Odor Activity Values (OAV) reported in Figs. 2 and 6 were
calculated by dividing the concentration of each compound by its odor
threshold (reported in Table 3) for every sample. The OAV were not
computed for norisoprenoids (since they are not quantified as μg/L, but
as relative areas), neither for the compounds with no odor threshold
reported in literature. All the samples collected during vessel storage (51
samples) were used to compute the averaged OAV for each compound
(showed in Fig. 2), as well as all the samples collected after bottle
storage (36 samples) were used to compute the averaged OAV for each
individual compound (showed in Fig. 6).
2.4. Sensory analysis
A descriptive analysis of samples was performed by a panel of 11
winemakers and wine experts familiarized with Chilean Sauvignon
blanc wines. The samples for sensory analysis were prepared as follow:
The three bottles (biological replicates) corresponding to the same
conditions (stored in the same kind of vessel and capped with the same
closure) were mixed in a single batch -after verifying that none of them
presented an organoleptic deviation-. The twelve resulting samples (four
different kinds of vessel, and three different closures for each one) were
tasted once by the panel, served at 12–14 ◦ C by using ISO official tasting
glasses (ISO 3591.1977), and labeled with a three-digit numeric code
stablished aleatorily. The order of tasting the samples was randomly
modified for each taster, to avoid any effect of fatigue. Four aromatic
attributes (aromatic intensity, typicality, vegetable scents, and fruity
scents) were scored by tasters using a 15 cm unstructured line (with an
expression denoting the intensity and direction above each end of the
line). The obtained scores of tasted wines from the individual panelists
were computed and standardized by using the software PanelCheck (v.
1.4.2).
2.5. Statistical analysis
All data are expressed as the mean ± standard deviation of three
biological replicates (from the three vessels of each type, both for the
results of vessel storage and those of bottle storage). Duncan’s test
(p < 0.05) was used for multiple comparisons and computed by using
InfoStat Software (v. 2018, Centro de Transferencia InfoStat, FCA,
Universidad Nacional de Córdoba, Argentina). The multivariate ana­
lyses (PCA and cluster analysis) were performed with the results of the
final wines (after vessel and bottle storages), using the same software
(InfoStat). The variables employed for the PCA and cluster analysis
correspond with the concentration of each individual volatile compound
as well as the total concentration of each chemical family (58 variables
in total), and they are listed in the Table 3. Graphs were depicted by
using GraphPad Prism 9 software (GraphPad Software, San Diego, CA).

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Table 3
Variables employed for the multivariate statistics and labeling used for the loading plot of the principal component analysis (Fig. 4). Odor threshold values for in­
dividual compounds employed to calculate the OAVs (Figs. 2 and 6), and the matrix employed to assess the odor threshold according to the literature.
Label Compound OdorThreshold Descriptor Matrix Ref.
(ppb)

1 ethyl acetate 12,270 Solvent, fruity, sweetish White wine 10 % (v/v) A

2 ethyl butyrate 20 Fruity, apple 10% (w/w) aqueous ethanol solution B
3 ethyl-2-methylbutyrate 0.2 Fruity 40% ethanol A
4 ethyl isovalerate 3 Fruit 10% (v/v) aqueous ethanol solution, pH 3.5 adjusted with tartaric acid B
5 isoamyl acetate 50 Banana, fruity 12.5% (v/v) hydroalcoholic solution, 5 g/L tartaric acid, pH adjusted to 3.2 B
with NaOH
6 methyl hexanoate n.f.
7 ethyl hexanoate 45 Apple peel, fruit 12.5% (v/v) hydroalcoholic solution, 5 g/L tartaric acid, pH adjusted to 3.2 B
with NaOH
8 hexyl acetate 400 Apple, cherry, pear, flower 12.5% (v/v) hydroalcoholic solution, 5 g/L tartaric acid, pH adjusted to 3.2 B
with NaOH
9 ethyl 2 hexenoate n.f.
10 methyl octanoate n.f.
11 ethyl octanoate 5 Sweet, ripe banana, pear White wine B
12 ethyl nonanoate 850 Fruity, fatty acids, perfumed, White wine at 10% (v/v) A
sweetish
13 ethyl decanoate 200 Fruity, floral 10% (v/v) aqueous ethanol solution, pH 3.5 adjusted with tartaric acid B
14 isoamyl octanoate n.f.
15 diethyl succinate n.f.
16 ethyl 9 decenoate n.f.
17 ethyl phenylacetate 73 Honey, sweet Red wine C
18 β-phenethyl acetate 1510 Roses, honey, apple, sweetish White wine at 10% (v/v) A
19 ethyl dodecanoate 800 Soapy, estery 23% (v/v) Grain whisky A
20 ethyl tetradecanoate n.f.
21 diethyl di malate n.f.
22 ethyl hexadecanoate n.f.
23 isobutanol 40,000 Alcohol 10% (w/w) Ethanol A
24 isoamyl alcohol 40 Whiskey, malt, burnt 14% (v/v) ethanol solution adjusted to pH 3.5 with tartaric acid B
25 hexanol 1100 Resin, flower, green, cut grass 10% (v/v) aqueous ethanol solution, pH 3.5 adjusted with tartaric acid B
26 E-3-hexenol 15,000 Bitter, green leaves Beer A
27 Z-3-hexenol 1000 Green, cut grass 14% (v/v) ethanol solution adjusted to pH 3.5 with tartaric acid B
28 2-phenylethanol 14 Honey, spice, rose, lilac 10% (v/v) aqueous ethanol solution, pH 3.5 adjusted with tartaric acid B
29 hexanoic acid 420 Sweat 11% (v/v) ethanol, 7 g/L glycerin, 5 g/L tartaric acid, pH adjusted to 3.4 with B
NaOH
30 octanoic acid 500 Sweat 11% (v/v) ethanol, 7 g/L glycerin, 5 g/L tartaric acid, pH adjusted to 3.4 with B
NaOH
31 decanoic acid 1000 Rancid, fat 11% (v/v) ethanol, 7 g/L glycerin, 5 g/L tartaric acid, pH adjusted to 3.4 with B
NaOH
– limonene 10 Fruity, citrus, citrus peel Water A
32 nerol oxide 100 Floral Wine D
33 linalool formate n.f.
34 linalool 25.2 Fruity, citrus, floral, lavender 10% (v/v) aqueous ethanol solution, pH 3.5 adjusted with tartaric acid B
35 hotrienol 110 Floral, fennel, ginger Unknown E
36 α-terpineol 250 Floral, lilac, pine 11% (v/v) ethanol, 7 g/L glycerin, 5 g/L tartaric acid, pH adjusted to 3.4 with B
NaOH
37 citronellol 100 Citronella, rose, green 10 % ethanol (w/w) F
38 vitispirane 1 800 Floral, fruity, woody Wine G
39 vitispirane 2 800 Floral, fruity, woody Wine G
40 ionene n.f.
41 TDN 2 Petrol Wine H
42 β-damascenone 0.05 Apple, fruity, flowery 10 % hydroalcoholic solution, pH 3.2 B
43 3-(Methylthio)-1- 1000 Sweet, potato 10% (v/v) aqueous ethanol solution, pH 3.5 adjusted with tartaric acid B
propanol
44 2-methylthiolan-3-one n.f.
45 Total ethyl esters
46 Total acetate esters
47 Total other esters
48 Total esters excluding
EtAc
49 Total esters
50 Total C6 alcohols
51 Total alcohols
52 Total C6 compounds
53 Total acids
54 Total terpenes
55 Total norisoprenoids
56 Total thiols
57 Total VOCs excluding
EtAc
58 Total VOCs

Label: code of every variable employed in the PCA loading’s chart (Fig. 4) n.f.: not found. Ref: bibliographic reference for the reported odor threshold. A: (Miller, 2019)
B: (Benkwitz et al., 2012) C: (Tat, Comuzzo, Battistutta, & Zironi, 2007) D: (Marais, 1983) E: (Baron, Prusova, Tomaskova, Kumsta, & Sochor, 2017) F: (Black, Parker,
Siebert, Capone, & Francis, 2015) G: (Simpson, 1978) H: (Sacks et al., 2012).

6
C. Ubeda et al.
Fig. 3. Scores obtained for each wine at the end of bottle aging during principal component analysis (PCA). Gray globes correspond to the two main groups obtained
by a cluster analysis using the same data as PCA. The variables employed for the PCA and clusters analyses are shown in Table 3.
3. Results and discussion
3.1. Evolution of volatile compounds during six months of storage in the
different types of vessels
The analysis of volatile compounds (VOCs) of the wines stored in the
different vessels throughout the storage period (accounting for six
months) allowed the determination of 45 volatile compounds, including
21 esters, 5 alcohols, 3 acids, 8 terpenes, 5 norisoprenoids, and 2 thiols.
The concentration of each individual VOC for every sampling point (t0:
initial wine, t1: 1.5 months of vessel storage, t2: 3.0 months of vessel
storage, t3: 4.5 months of vessel storage, and t4: 6 months of vessel
storage) is shown in Table 1S (supplemental data).
Table 1 shows the total VOC contents grouped by chemical family at
every sampling point, where it can be observed that the initial wine
(sampled from the raw vat) contains a greater concentration of VOCs for
all the chemical families. This fact is related to a loss of VOCs during the
pumping of wines to fill the different types of vessels, either due to loss
by evaporation or by oxidation associated with aeration and the corre­
sponding oxygen dissolution (Baiano et al., 2015; Ribéreau-Gayon,
Glories, Maujean, & Dubourdieu, 2006a). After such initial loss, a
gradual increase was observed for the VOC chemical families
throughout vessel aging, which corresponded to a trend previously re­
ported during a trial in which white Muscat wine was aged for 90 days
(Călugăr et al., 2020). After a month and a half of storage (t1), wines
from CYL showed the highest contents of total acids and the highest
contents of terpenes when compared with wines from CUB. After three
months of storage (t2), CYL wines still showed the highest contents of
total acids. In addition, at the same sampling time, they showed higher
contents of total ethyl esters than OVO as well as higher contents of total
acetate esters when compared with CUB wines. After four and a half
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Food Research International 156 (2022) 111178
months of storage (t3), the differences among wines stored in different
vessels were amplified. Wines stored in OVO showed greater concen­
trations than CUB for all of the analyzed chemical families other than
thiols. Given that both types of vessels are made of polyethylene with the
same properties, these results seem to indicate that -at least in the case of
polyethylene- the shape of the tanks has a greater impact on the VOCs
than the material of which they were made. The main difference
observed at t3 lies in the concentration of ethyl acetate. This ethyl ester is
usually present in wines above its odor threshold (12000 µg/L),
contributing to a “fruity” perception when present in low amounts and
to a “volatile acidity” perception when present at higher concentrations.
Its natural tendency during storage is to decrease (Patrianakou &
Roussis, 2013), but the concentration present in the wines from the oval-
shaped polyethylene tanks decreased until t2, increased significantly
until t3, and finally decreased again until t4 (Table 1S). Regardless of the
type of vessel, the decreases in the concentrations of ethyl esters were
less intense than those observed for acetic esters, which diminished to a
greater extent. The higher lability of acetate esters compared to ethyl
esters during storage agrees with previous reports (Makhotkina & Kil­
martin, 2012). Interestingly, the decreasing trend of the acetate esters in
the wine stored in CUB was barely different than in the other vessels. The
amount of acetate esters decreased in all of the vessels until t1-t2, but in
t3 and t4, the amount increased except for the CUB tanks, in which the
acetate concentration continued to decrease. Moreover, at the same
sampling time, t3, wines from OVO showed the highest concentrations of
total norisoprenoids. These compounds are typical aging markers com­
ing from grape carotenoids in their free form and glycosylated; the latter
is released into the wine during fermentation and aging/storage via
enzymatic and nonenzymatic (acid hydrolysis) pathways (Mendes-
Pinto, 2009). It has been described that norisoprenoids increase their
presence in wine during aging, which is enhanced by heat and oxygen
C. Ubeda et al.
Fig. 4. Loadings of every variable obtained by the PCA. The labels used in this chart are decodified in Table 3.
(Cejudo-Bastante, Hermosín-Gutiérrez, & Pérez-Coello, 2013; Silva
Ferreira & Guedes De Pinho, 2004). Regarding terpenes, at t3, OVO
wines showed higher amounts than CUB wines. Terpenes are also iso­
prenoids coming from grape carotenoids present in the grapes in their
glycosidic form released in the wine in the same ways as norisoprenoids.
OVO tanks started the accumulation of norisoprenoids and terpenes
earlier than the other vessels, indicating that hydrolysis reactions could
be enhanced in that type of vessel. In addition, wines from the OVO and
CYL tanks showed higher contents of alcohols and acids than the other
vessels (CUB and JAR) as well as greater concentrations of total VOCs
than wines from the CUB tanks. In contrast, after six months of vessel
storage (t4), the differences among vessels smoothed out until no sta­
tistical significance was reached.
Two out of the eight families of volatile compounds determined,
specifically acids and alcohols, showed a statistical interaction between
the storage time and the type of vessel employed, which indicates that
all of the vessels did not have the same behavior through storage for
these families of volatiles. As shown in Fig. 1, where the entire vari­
ability of volatile compound contents (grouped by chemical family) is
shown, wines from JAR showed the least acid concentration variability
throughout the vessel storage period. In the same way, wines stored in
CYL and JAR vessels also showed lower variability of terpenes
throughout the storage time when compared with polyethylene tanks
(regardless of their shape). These results seem to indicate that poly­
ethylene tanks lead to more dispersion of the VOC content during the
first six months of wine storage in vessels. Among the chemical families
of volatiles reported in Table 1 and Fig. 1, volatile acids showed
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significant differences at three out of four sampling points. It has been
described that wine fatty acid contents depend mainly on the initial
must content and yeast metabolism during alcoholic fermentation
(Coetzee & Du Toit, 2015). However, under the conditions of the present
trial, the raw grapes were processed as a single batch; therefore, alco­
holic fermentation was performed in a single tank, and all of the vessels
were filled with the resulting wine. Thus, differences observed among
wines during storage should be due to a direct or indirect effect of the
vessel. Such an effect could be related to the isolation of this vessel from
external conditions and therefore the temperature variability and oxy­
gen exposition of wines throughout storage. It has been described that
winemaking without sulfite addition decreases the content of fatty acids
in wines during aging (Garde-Cerdán & Ancín-Azpilicueta, 2007; Pati,
Crupi, Savastano, Benucci, & Esti, 2020). Due to the consumption of
dissolved oxygen that takes place when SO2 is added to wine, it seems
quite logical to associate a greater content of dissolved oxygen with a
lower content of fatty acids, as reported by (Carien Coetzee et al., 2013).
Our results support this hypothesis since the wines stored in stainless-
steel tanks (an impervious oxygen material) had higher contents of
total acids after 1.5, 3.0, and 4.5 months of storage. Volatile acids were
better retained in the CYL tanks, mainly because the concentration of
decanoic acid remained constant (Table 1S). This medium-chain fatty
acid has been described in white wine as being more vulnerable to
degradation during storage when compared with hexanoic and octanoic
acids, either during short-term aging (Garde-Cerdán, Marsellés-Fonta­
net, Arias-Gil, Ancín-Azpilicueta, & Martín-Belloso, 2008; Rubio-Bretón
et al., 2018) or during longer periods in bottles (Fracassetti, Camoni,
C. Ubeda et al. Food Research International 156 (2022) 111178

Fig. 5. Concentrations of ionene, ethyl isovalerate,

and methyl hexanoate in wines after six months of
vessel storage followed by six months of bottle
aging. Bars correspond to the mean, and error bars
correspond to the standard deviation. Different
lowercase letters above bars indicate significant
differences (p < 0.05) among closures for wines
stored in the same type of vessel. Different capital
letters within bars indicate significant differences
(p < 0.05) among vessels for wines capped with the
same closure.

Montresor, Bodon, & Limbo, 2020). with the higher aromatic impact, meanwhile terpenes and thiols were
To better understand how the differences of the reported VOC pro­ expected to have low impact on the aromatic perception of wines.
files could affect the aromatic perception of wines, the averaged odor
activity values (OAV) of each compound were calculated. When the OAV
3.2. Profile of wine volatile compounds after aging in bottles by using
is lower than 1 indicates that the concentration of the volatile compound
different caps
is below its odor threshold and, therefore, it has no impact on the aro­
matic perception of wine. Thus, considering the wines during vessel
After the storage period in vessels, the wines underwent bottle aging
storage (Fig. 2), alcohols, esters, and acids correspond to the compounds
for six months by using three different types of caps: natural cork (NAT),

9
C. Ubeda et al.
Fig. 6. Averaged Odor Activity Values (OAV) of individual volatile compounds from the wines after bottle storage. The odor thresholds employed to calculate the
OAV are shown in Table 3. The dotted line indicates the OAV = 1.
synthetic cork (SINT), and screw cap (SCR). Table 2 shows the VOC
contents of wines after the bottle aging process grouped by chemical
family, and the data for each individual VOC are shown in the supple­
mental data (Table 2S).
When NAT was used as a cap, CYL wines showed the highest contents
for all of the studied families except for acetates (where CYL wines had
greater contents than CUB wines), C6 compounds, and thiols (showing
the same trend: CUB wines had the lowest contents). Using SINT as a
closure, wines stored in CYL showed the highest contents of ethyl esters,
other esters, total esters, and norisoprenoids. Moreover, for acetates,
alcohols, acids, and total VOCs, CYL wines showed higher contents than
OVO and JAR wines. CYL wines had higher contents of C6 alcohols than
JAR wines. Finally, there were no significant differences among the
wines stored in different vessels for C6 total compounds, terpenes, and
thiols when SINT caps were employed. When SCR was used as a cap,
there were no significant differences among vessels for most of the
studied families of VOCs, except for other esters (CYL wines showed
higher contents than OVO and JAR wines), C6 total compounds (CUB
wines showed higher contents than CYL wines) and acids (JAR wines
showed lower contents than CYL and CUB wines). Looking at the results,
it seems that using stainless steel tanks increases the content of VOCs in
the resulting wines, especially when aging in bottles is performed using
NAT or SINT caps, while the use of SCR smooths out the differences
among wines stored in different vessels. In contrast, the use of NAT caps
seems to emphasize the effect of the vessel employed during aging since
all of the studied families of VOCs show significant differences among
wines from the different types of vessels. The reported greater concen­
tration of VOCs for wines stored in CYL vessels agrees with previous
works in which different types of vessels were evaluated during alco­
holic fermentation and aging on lees (Gil i Cortiella et al., 2021, 2020).
The bottle oxygen intake depends strongly on the type of closure.
According to the specifications of the closures employed during this
trial, SINT is expected to allow the highest oxygen ingress after bottling,
followed by NAT and SCR (Furtado et al., 2021). Moreover, the
employment of NAT and SINT corks represent and additional intake of
oxygen during capping, due to a plunger effect when the cork is inserted
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Food Research International 156 (2022) 111178
in the neck of the bottle. This plunger effect does not exist in the case of
screw caps. However, the headspace of the wines capped using screw
cap is greater than those wines capped with NAT and SINT corks, due to
the volume occupied by the cork itself. For the wines stored in CYL
tanks, no significant differences among the different types of caps were
observed for most of the studied families of VOCs, except for C6 com­
pounds (where wines capped with SINT showed higher contents than
wines capped with SCR) and norisoprenoids (where a trend is observed
with SCR wines showing the highest contents and SINT wines showing
the lowest). Giuffrida de Esteban et al. (2019) also observed greater
contents of norisoprenoids in wines bottled by using screwcaps than in
those bottled by using natural corks. In contrast, He et al. (2013) found
that using a screw cap with high oxygen permeability led to a greater
concentration of β-damascenone. According to the reported results, the
trend for norisoprenoids among bottle closures seems to indicate that
the lower the oxygen exposure is, the higher the norisoprenoid content,
which could be explained by oxidative degradation (Silva Ferreira &
Guedes De Pinho, 2004). In addition, an adsorption effect of 1,1,6-tri­
methyl-1,2-dihydronaphthalene (TDN) by cork has been described
(Tarasov et al., 2019), which could also explain the higher contents of
such compounds when bottles were capped with SCR.
Regarding the wines stored in OVO tanks, there were no differences
among the caps used during bottle aging for acetates, other esters, C6
compounds, acids, and thiols. In contrast, for total esters, alcohols,
norisoprenoids, and total VOCs, wines aged using SCR showed the
highest contents. Moreover, for ethyl ester and terpene contents, wines
aged with SCR had higher contents than those aged using SINT. Finally,
SCR wines had higher contents of C6 alcohols than NAT wines. Once
again, in general terms, it seems that the use of SCR closures, which
prevent oxygen intake throughout bottle storage, leads to wines with
higher contents of volatile compounds, which could be related to lower
degradation by oxidation pathways.
For the wines stored in CUB tanks, there were no significant differ­
ences among caps for acetates, total esters, C6 alcohols, and terpenes.
However, SCR wines showed the greatest contents of ethyl esters, nor­
isoprenoids, and total VOCs. A higher content of ethyl esters in wines
C. Ubeda et al. Food Research International 156 (2022) 111178

capped with SCR could be expected since partial adsorption of ethyl

Fig. 7. Results for sensory analysis of wines after six months of vessel storage
and six months of bottle storage.
octanoate and ethyl decanoate by natural and technical cork stoppers
has been described (Capone, Sefton, & Hoj, 2003). This effect can be
observed in Table 2S, not only in the case of such esters but also for most
of the analyzed ethyl esters, regardless of the vessel employed, although
the results were not statistically significant in all the cases. Moreover, for
other esters and alcohols, SCR wines contained more alcohols and other
esters than NAT wines. For C6 compounds, acids, and thiols, SINT and
SCR wines had higher contents than NAT wines.
Regarding wines from JAR, there were no significant differences for
acetates, other esters, C6 alcohols, C6 compounds, alcohols, acids, thiols,
and total VOCs. In contrast, for ethyl esters, total esters, terpenes and
norisoprenoids, wines capped with SCR showed the highest contents,
which could be related to either lower degradation by oxidation or lower
adsorption by the cork.
To better understand the combined effect of vessels employed during
storage and bottle closure during aging in the bottle, multivariate sta­
tistical analysis (consisting of principal component analysis (PCA) and
cluster analysis) was applied using the variables listed in Table 3, and
those results are summarized in Figs. 3 and 4. The cluster analysis
grouped samples stored using CYL tanks in addition to samples with SCR
closures (regardless of the vessel employed during winery storage), and
they showed higher scores for PC1. In contrast, wines stored in OVO,
CUB, and JAR vessels with NAT and SINT caps belong to a different
cluster, showing lower values for PC1. Moreover, wines capped with
SINT showed the greatest scores for PC2. These results seem to indicate
that using SCR closures had similar effects to storing the wines in CYL
tanks, and the resulting wines differed from those stored using alter­
native vessels capped with either NAT or SINT closures. Somehow these
results indicate that the singularity of the VOC profile of wines stored in
vessels alternative to the conventional stainless-steel tanks is lost when
wines are capped using SCR, which could be valuable information for
winemakers, helping them to better understand how to maximize the
singularity of their brands. Regarding the loadings chart (Fig. 4), ionene
(40), a norisoprenoid that corresponds with a reduced form of TDN,
showed an obvious different behavior when compared with the other
variables, with a great weight differentiating wines aged in vessel al­
ternatives to stainless steel except when they are capped using screw­
caps. Such a compound has been previously described in commercial
white and red wines (Gürbüz, Rouseff, & Rouseff, 2006; Mendes-Pinto,
2009; Somkuwar et al., 2020) and is considered a key aromatic com­
pound in wines from cultivars such as Riesling (Winterhalter, 1991),
with a “kerosene/petrol like” descriptor. Moreover, ionene is employed
as a precursor to synthesize the TDN standard (Dobrydnev et al., 2020),
which is also indicative of the relationship between both molecules.
Fig. 5 shows the ionene contents of matured wines (after six months of
vessel storage followed by six more months of bottle aging). For wines
stored in OVO, CUB, and JAR vessels, wines capped with natural cork
show greater contents of ionene when compared with the other closures.
In contrast, for wines stored in CYL tanks, wines capped with SCR had
the lowest amounts, while those capped with SINT showed the highest.
It seems that using vessels that allow oxygen to permeate through en­
hances the ionene content of the resulting wines, while using stainless
steel tanks (impervious to oxygen) reduces its content. Moreover, for
wines stored in CYL tanks, using closures with higher oxygen intake
rates also seems to enhance the ionene content. Thus, the content of this
compound in finished wines seems to be related to oxygen exposure
during wine aging. The results shown in Table 2S seem to establish a
relationship between ionene and TDN during aging: when ionene in­
creases, TDN decreases and vice versa; therefore, it could be hypothe­
sized that the existence of an equilibrium balance between them is
encouraged by oxidation. This point could be interesting because the
presence of TDN is desired is some wines (e.g., Riesling) because it is a
key aroma of its typicality. However, in more conventional wines, an
excessive concentration of TDN could be considered an off-flavor or an
unpleasant scent that could be rejected by consumers (Mendes-Pinto,

11
C. Ubeda et al.
Fig. 8. Heatmap for the % variation of individual VOCs of wines aged in different types of vessels throughout aging in bottles using different caps. (This figure
includes the VOCs whose variation is between − 100 and + 100%).
2009). Given that global warming is linked to an increase in radiation
and that this triggers the synthesis of TDN in berries (Marais, van Wyk, &
Rapp, 2017), the employment of vessels other than CYL, with more
permeability to oxygen combined with the selection of a cork cap to
favor the ionene (citric/solvent) form compared to TDN (kerosene/
petrol), should be considered, thus decreasing the amounts of this nor­
isoprenoid in the resulting wines.
As done with the wines during the vessel storage, the averaged OAV
of each compound were calculated for matured wines in bottle, those
results are shown in Fig. 6. During the bottle storage, the OAV of the
compounds β-phenethyl acetate (with roses, honey, and apple de­
scriptors), decanoic acid (with rancid/fat descriptors), and hexyl acetate
(with fruity and floral descriptors) fall below 1, thus, their impact on the
aromatic perception of wines is expected to be lower when compared
with wines before bottling. In contrast, the OAV of nerol oxide (with
floral descriptors) and ethyl isovalerate (with fruit descriptors)
increased until reach values higher than 1 after bottle storage, which
indicates that they have a higher impact on the aromatic perception
after bottle ageing. Despite such differences, the compounds 2-phenyle­
thanol (related with honey, spice, and floral scents) and isoamyl alcohol
(related with whiskey, malt, and burnt scents) remain as the compounds
with the highest OAV and, therefore, they are expected to be the most
impactful compounds on the aromatic perception of wines after bottle
ageing.
Given that it is not possible to know the OAV of each analyzed
compound, due firstly to the fact that several compounds have not
known odor thresholds in wine (or wine-like solutions), and secondly, to
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Food Research International 156 (2022) 111178
the fact that some of the compounds were not quantified as true con­
centrations (e.g. norisoprenoids, expressed as relative areas), a sensory
analysis of matured wines was performed, and the results are summa­
rized in Fig. 7. The aromatic intensity of wines from all the vessels are
similar. However, for wines stored in OVO, the wines capped with
natural cork showed lower intensity when compared with those capped
with screw cap and synthetic cork. Regarding varietal typicality, wines
stored in CYL, OVO, and CUB vessels showed the same trend, with the
lower typicality for the wines capped with natural cork, although it is
not statistically significant. Besides, for the wines stored in JAR vessels,
wines capped with screw caps showed the highest values among clo­
sures. Considering vegetable scents, each kind of vessel seem to interact
by a different way with the employed closures, but without showing
statistical differences. Finally, regarding fruity scents, the wines stored
in CYL seem to be fruitier than the wines stored in the other kinds of
vessels, which agree with its higher content of esters. Moreover, for the
wines stored in CYL tanks, the wines capped with synthetic cork were
rated as fruitier than those capped with natural cork.
3.3. Interaction between the vessel used during winery storage and the
closure used during aging in bottles
The presented results seem to indicate that wine evolves differently
during aging in bottles as a function of the vessel in which it is stored. To
better understand such interactions, the variation in VOCs between the
wines at the end of vessel storage (t4) and the wines at the end of bottle
aging was analyzed. In general, terms, the profile of VOCs was
C. Ubeda et al.
Fig. 9. Percentage of variation of individual VOCs of wines aged in different types of vessels throughout aging in bottles using different caps. (This figure includes the
VOCs whose variation is greater than 100%).
maintained throughout aging in bottles, although E-3-hexenyl acetate,
E-4-hexenyl acetate, isoamyl decanoate, limonene, and trans-nerolidol
completely disappeared during this process. In contrast, ethyl iso­
valerate and methyl hexanoate were only detected in wines after aging
in the bottle process; thus, both compounds should be formed during
bottle storage. For wines stored in OVO, CUB, and JAR vessels, wines
capped with SCR showed the highest concentrations of ethyl isovalerate
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Food Research International 156 (2022) 111178
(Fig. 5), while no significant differences were found among closures for
wines stored in CYL, which agrees with results reported by Makhotkina
& Kilmartin (2012), showing a significant increase in ethyl isovalerate in
Sauvignon Blanc wines during storage in bottles capped with screw caps.
In addition, for wines capped with SINT, wines from OVO vessels
showed lower contents of ethyl isovalerate than CYL and CUB wines.
This result again suggests that the shape of vessels could influence the
C. Ubeda et al.
volatile profile of wines since OVO and CUB vats are both made up of the
same type of polyethylene but differ in shape. The methyl hexanoate
concentration (Fig. 5) showed differences among vessels only for the
wines capped with natural cork and differences among closures just for
wines stored in OVO vessels. When natural cork was employed, CYL
wines had higher concentrations of methyl hexanoate than OVO and
JAR wines. For wines stored in OVO vessels, SCR closures had the
highest concentrations of methyl hexanoate.
The variation for each compound from the end of vessel storage (t4)
to the end of bottle aging was calculated (%), and those results are
shown in Fig. 8 (for those VOCs showing variations between − 100%
and + 100%) and Fig. 9 (for those VOCs showing variations higher than
100%). The heatmap of Fig. 8 allows us to realize, at a glance, that wines
stored in CYL vessels as well as wines capped using SCR had higher
increasing rates and lower decreasing rates for most of the analyzed
compounds. In addition, acetate esters tend to decrease (dramatically, in
most cases), while esters other than acetates remain constant or increase
during bottle aging. Moreover, the behavior of isobutanol seems to be
vessel dependent since wines stored in CUB showed higher increasing
rates. Finally, for vessels other than CYL, the decrease in ionene was
quite lower when NAT was used for closure according to its higher
amounts found in the wines after aging in the bottle period.
Regarding compounds with variation rates exceeding 100% (Fig. 9),
the trends observed for TDN, vitispirane A, and vitispirane B (all of them
considered norisoprenoids) among bottle closures were remarkable.
Wines capped with SCR had the highest increasing rate of nor­
isoprenoids during bottle aging, while those capped with SINT had the
lowest. Considering the features of the closures employed during this
trial, these results seem to indicate that higher oxygen exposure during
bottle aging leads to a lower increase in norisoprenoids. It is also notable
that the increases of diethyl succinate and diethyl malate were notice­
ably lower for wines stored in CUB vats capped with NAT cork. Unex­
pectedly, diethyl succinate, a typical aging marker that increases during
bottle storage (Makhotkina & Kilmartin, 2012), decreased after this 6-
month period. In contrast, ethyl malate increased in all cases during
bottle storage, according to the results reported in the literature
(Makhotkina & Kilmartin, 2012). For ethyl decanoate, the use of SCR
ensures a higher increasing rate for wines stored in CYL, CUB, and JAR
vessels and a lower decreasing rate for OVO wines. Moreover, ethyl
decanoate, ethyl dodecanoate, and ethyl hexadecanoate rates seem to be
vessel dependent. Ethyl decanoate and ethyl dodecanoate contents were
maintained for wines stored in OVO and capped with SCR, but they
dropped during bottle aging when NAT or SINT was used as a closure. As
previously mentioned, these compounds tend to be adsorbed in the cork,
and the capacity of adsorption by the cork is proportional to the ester
chain length (Capone et al., 2003). In addition, wines stored in CYL
(regardless of the closure) and the combination of CUB-SCR showed
higher increasing rates for both compounds. For ethyl hexadecanoate,
wines stored in OVO vessels show the lowest increasing rates. Finally,
nerol oxide was noticeably the compound that showed the highest in­
creases during bottle aging, and those increases seemed to be favored by
the use of SCR closures, especially in the case of wines from OVO and
JAR vessels. While most terpenes naturally tend to decrease during
aging, other terpenes, such as nerol oxide, increase (Oliveira, Oliveira,
Baumes, & Maia, 2008); however, the perception odor threshold of the
oxidized form is higher than that of the parent terpene.
4. Conclusion
In view of the presented results, it could be concluded that the vessel
employed during storage impacts the volatile composition of the
resulting wines. Wines stored in conventional stainless-steel tanks
contain higher amounts of most of the volatile compounds analyzed.
Moreover, capping bottles with screwcaps leads to wines with higher
concentrations of volatile compounds. In addition, an interaction be­
tween the vessel used for wine storage and the bottle closure was
14
Food Research International 156 (2022) 111178
observed: when vessels other than stainless steel were used during
storage, the volatile profiles of the resulting wines were distinguishable
as long as the employed closure was not screw-cap. Therefore, the se­
lection of vessels and closures during wine maturation could be
employed as a tool by winemakers to modulate wine features and could
be a helpful strategy to mitigate the side effects of uncontrolled elements
such as climate change.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
This work was supported by ANID-Chile (Project FONDECYT
11160510, FONDECYT 1210844, and FONDEQUIP EQM130129). The
authors thank Miguel Torres Chile for the winery facilities and sample
supply. Finally, Dr. Cristina Ubeda is thankful to the VI Plan Propio de
Investigación y Transferencia of the University of Seville for her current
research contract (Contract number USE-18644-Z).
Appendix A. Supplementary material
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.foodres.2022.111178.
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