Food Control 18 (2007) 521–529

www.elsevier.com/locate/foodcont

EVect of storage time and container type on the quality

of extra-virgin olive oil
¤
Ana Isabel Méndez, Elena Falqué
Química Analítica, Depto. Química Analítica y Alimentaria, Facultad de Ciencias, Universidade de Vigo, As Lagoas s/n, 32004 Ourense, Spain

Received 10 April 2005; received in revised form 30 December 2005; accepted 30 December 2005

Abstract

Four commercial samples of extra-virgin olive oil have been analysed in order to evaluate the inXuence of storage time on quality. The
following parameters were determined after 3 and 6 months of storage: acidity, peroxide index, absorption coeYcients K270 and K230, per-
centage of humidity, impurity content (%), phenols content, iodine index, saponiWcation index, colour index and fatty acid content. At the
same time, the eVects of container type on the deterioration in quality were studied. Each olive oil was stored in Wve diVerent containers at
room temperature with the same surface area of exposition to air and light: clear PET bottle, PET bottle (covered with Al foil), glass bot-
tle, tin, and Tetra-brik®. The results showed a gradual loss of quality during storage, especially in plastic or glass bottles. The best contain-
ers for commercial packing of extra-olive oil were tin and Tetra-brik®.
© 2006 Elsevier Ltd. All rights reserved.

Keywords: Extra-virgin olive oil; Storage time; Container; Chemical composition

1. Introduction in the bottle. Thus, it is necessary to care for each step of

Among the diVerent categories of olive oil, the “extra-
virgin olive oil” is outstanding in gastronomic, nutritional,
therapeutic and economic importance. The other categories
are generally used for cooking and in salads, but have less
taste and aroma.
Extra-virgin olive oil is considered to be the best olive oil
for its organoleptic characteristics, for its stability and its
chemical composition. It is the juice of the olive that is har-
vested at optimum maturity and correctly processed. It is
practically the only vegetable oil that can be consumed
directly in its raw state and contains important nutritional
elements (fatty acids, vitamins, etc.). It should have an orga-
noleptic score of 76.5 and a maximum acidity of 1° (EC,
1991, 1997).
This excellent quality of extra-virgin olive oil is the cul-
mination of a process that begins with the tree and Wnishes
*
Corresponding author. Tel.: +34 988 387081; fax: +34 988 387001.
E-mail address: efalque@uvigo.es (E. Falqué).
the process and of the factors that can aVect its commercial
life (oxygen, light, temperature, metals, etc.) leading to a
deterioration in quality as a consequence of oxidative and
hydrolytic degradations (Psomiadou & Tsimidou, 2002a,
2002b). Similar to other products that are produced in a
limited period of time, but that are consumed throughout
the year, it must be stored, and these storage and packing
conditions are going to determine the commercial life of the
olive oil (Hrncirik & Fritsche, 2005; Kiritsakis & Dugan,
1984; Zanoni, Bertucciolo, Rovellini, Marotta, & Mattei,
2005). In particular, among the natural antioxidants, phe-
nolic compounds, -tocopherol and -carotene, are
reported to play a key role in preventing oxidation and
have been already correlated to the storage stability of vir-
gin olive oils (Baldiolo, Servili, Perreti, & Montedoro, 1996;
Rahmani & Csallany, 1998). The eVect of some storage
conditions (in darkness, diVused room light or direct sun-
light, at room or elevated temperature, exposure to air and
air/light, etc.) and/or packaging material (into glass and
polyethylene plastic bottles, into colourless or green bottles,

0956-7135/$ - see front matter © 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.foodcont.2005.12.012
522 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529
into tins, etc.) on olive oil quality (Murillo-Ramos, Bonilla-
Polo, González-Bonillo, & Sanz-Pérez, 1997; Naz, Siddiqi,
Sheikh, & Sayeed, 2005; Paganuzzi, De Lorgi, & Malerba,
1997), on olive marc oil quality (Méndez & Falqué, 2002),
and on extra-virgin olive oil quality (Caponio, Bilancia,
Pasqualone, Sikorska, & Gomes, 2005; de Leonardis &
Macciola, 1998; Procida & Cichelli, 1999) was studied by
several authors. The changes in oil quality are also reXected
in the standardized quality indices, oxidative stability and
tocopherol levels with the storage time (Gutiérrez & Fern-
ández, 2002). However, other predictive studies shown that
the stability of extra-virgin olive oil was not signiWcantly
inXuenced by diVerent controlled bottling, transport and
storage conditions in supermarkets (Pagliarini, Zanoni, &
Giovanelli, 2000).
Commonly, extra-virgin olive oil is usually packaged in
glass, tin or plastic bottles. The primary advantages for the
two Wrst ones are its impermeability to gases, but the glass
and plastic bottles had some disadvantages such as to
favour the photo-oxidation. This study was set up to inves-
tigate the change in extra-virgin olive oil quality, as a func-
tion of type of container and storage time, based on the
analysis of parameters such as acidity, peroxide index,
coeYcients K270 and K232, iodine index, colour index,
saponiWcation index, impurity, humidity and volatile mate-
rials, phenol compounds and fatty acids.
2. Materials and methods
Four commercial extra-virgin olive oils have been
selected: two of maximum acidity 0.7° (A1 and A2) and two
others of maximum acidity 0.5° (A3 and A4). And Wve con-
tainers were evaluated: plastic bottle (transparent), opaque
plastic bottle (covered with Al foil), glass bottle (transpar-
ent), tin, and Tetra-brik Aseptic®.
The olive oils were acquired in a supermarket so that the
amount of each variant selected had the same expiry date
and a homogenous sample could be obtained. All of the
selected olive oils had an expiry date exceeding the maxi-
mum duration of this investigation.
The total amount of each olive oil was emptied into a
sterile recipient for homogenisation and, in the minimum
possible time, was transferred without headspace to the Wve
containers studied in duplicates. Each of the oils was
poured into 330 mL poly(ethylene) terephtalate (PET)
transparent or covered, transparent glass, tin and Tetra-
brik aseptic® bottles with a surface area of 250 cm2 exposed
to air and light. The PET, obtained from the bottles of min-
eral water, was washed several times with distilled water
and dried. The glass, tin and plastic-coated paperboard
laminate containers, obtained from the bottles of soft
drinks, were sterilized. The closed bottles were placed in the
centre of a metallic shelf in a chamber with glass windows
at room temperature (20–22 °C) and in an adequate space
and separation to ensure equalized exposure to air and light
(natural and Xuorescence lamps). These storage conditions
were selected to simulate the real conditions in a market
place (illumination 10–12 h/day).
The olive oils were analysed at the time of purchase and
packing and after 3 and 6 months of storage at room tem-
perature (the series of bottles were stored without opening
for these times). The chemical and physical parameters
(acidity, peroxide index, absorption coeYcients in UV at
232 and 270 nm, iodine index, humidity, impurity, colour
index, saponiWcation index and fatty acid content) were
analysed, in triplicate, following the analytical methods
described in Regulations EEC/2568/91 and EEC/2472/97 of
the European Union Commission, and the phenol content
was determined according to the method proposed by
Satue, Huang, and Frankel (1995).
3. Results and discussion
To determine the eVect of the container type during the
storage time on the oil quality, the results of each parame-
ter were compared with the values obtained for the samples
analysed immediately after opening the original cans
(controls).
The values of the initial acidity of the extra-virgin olive
oils studied are below the maximum levels established by
the Regulations EEC/2568/91 and EEC/2472/97 of the
European Union Commission.
After storing the samples for 3 months (Table 1), a simi-
lar slight increase in acidity in the Wve types of container
was observed, although this was less marked in a plastic-
coated paperboard laminate and tin. After 6 months the
increase in acidity in all the containers was conWrmed, but
to a lesser degree in a plastic-coated paperboard laminate,
followed by tin can and glass bottle. The plastic bottle
appears to be the container in which the hydrolytic pro-
cesses of the glycerides was most intense, which could be
related to the permeability of the container to oxygen and
light, and less intense in the opaque plastic container (iso-
lated from the light) than in the normal transparent con-
tainer. Although the glass bottle does not allow the
penetration of gases, it is sensitive to the action of light on
the fatty acids, which also produces an increase in acidity.
The evolution of this chemical parameter shows slightly
lower values in the olive oils stored in a plastic-coated
paperboard laminate than in tin containers. These results
agree with the study performed by TawWk and Huygheba-
ert (1997) during 2 months that conWrmed the increase of
acidity in olive oil over time.
The initial peroxide index of the olive oils analysed
(Table 1) is between 18.3 and 19.7 meq O2/kg being lower
than the maximum values indicated by the EEC Regula-
tions. After 3 months of storage it can be seen that oxida-
tion is in advanced phases, due to the sensibility of extra-
virgin olive oil to photo-oxidation, although this is less
notable in the A2 and A3 oil samples stored in a plastic-
coated paperboard laminate and tin, as the natural pig-
ments of the extra-virgin olive oil (chlorophylls) in the
absence of light act as antioxidants, acting synergistically
 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529 523

Table 1
Evolution of the acidity and peroxide index of extra-virgin olive oil during the storage time and in diVerent containers
Container Storage time (month) Extra-virgin olive oil samples
A1 § S.D.a A2 § S.D. A3 § S.D. A4 § S.D.
Acidity (% oleic acid)
0 0.31 § 0.0003 0.39 § 0.0004 0.30 § 0.0003 0.25 § 0.0003
Plastic 3 0.36 § 0.0004 0.43 § 0.0004 0.39 § 0.0027 0.30 § 0.0010
6 0.45 § 0.0008 0.49 § 0.0005 0.46 § 0.0009 0.38 § 0.0014
Opaque plastic 3 0.36 § 0.0089 0.43 § 0.0025 0.36 § 0.0000 0.29 § 0.0005
6 0.44 § 0.0004 0.48 § 0.0005 0.45 § 0.0013 0.38 § 0.0007
Glass 3 0.35 § 0.0008 0.42 § 0.0022 0.36 § 0.0008 0.29 § 0.0003
6 0.44 § 0.0008 0.45 § 0.0009 0.45 § 0.0004 0.37 § 0.0007
Tin plate 3 0.35 § 0.0094 0.39 § 0.0016 0.33 § 0.0003 0.28 § 0.0010
6 0.44 § 0.0008 0.45 § 0.0005 0.42 § 0.0004 0.34 § 0.0006
Tetra-brik 3 0.34 § 0.0003 0.39 § 0.0004 0.32 § 0.0006 0.28 § 0.0010
6 0.41 § 0.0011 0.41 § 0.0011 0.41 § 0.0008 0.33 § 0.0003
Peroxide index (meq O2/kg oil)
0 19.7 § 0.09 19.0 § 0.12 18.6 § 0.23 18.3 § 0.08
Plastic 3 16.8 § 0.16 23.3 § 0.36 23.8 § 0.99 12.2 § 0.10
6 25.5 § 0.09 34.8 § 0.08 30.0 § 0.04 20.5 § 0.49
Opaque plastic 3 17.4 § 0.29 20.1 § 0.13 20.5 § 0.10 13.8 § 0.06
6 21.4 § 0.08 14.5 § 0.15 19.2 § 0.02 15.5 § 0.05
Glass 3 22.1 § 0.08 20.2 § 0.04 22.4 § 0.19 17.5 § 0.07
6 26.9 § 0.01 23.4 § 0.01 22.1 § 0.08 21.6 § 0.07
Tin plate 3 21.4 § 0.07 19.7 § 0.18 18.7 § 0.28 17.6 § 0.13
6 26.3 § 0.07 23.7 § 0.03 23.1 § 0.01 16.4 § 0.15
Tetra-brik 3 22.9 § 0.09 19.2 § 0.08 18.7 § 0.08 17.4 § 0.01
6 23.4 § 0.29 21.2 § 0.11 21.8 § 0.03 16.6 § 0.11
a
S.D.: standard deviation of three replicates.

with the phenol antioxidants (Interesse, Ruggiero, & Vita-
gliano, 1971), inhibiting the initiation stage of auto-oxida-
tion. An increase in the peroxide index (propagation phase)
is produced in all the samples at 6 months, as, once auto-
oxidation is started, it does not stop until all the free radi-
cals that are formed are inactivated (Kiritsakis, 1992). The
less signiWcant evolution of the peroxides during the period
of analysis is very similar in the plastic-coated paperboard
laminate and in the tin container.
The opaque plastic, as in the two previous types of con-
tainer, protects the olive oil from the light, but its perme-
ability to oxygen accelerates the auto-oxidation process,
acting as a catalyst. The oxidation reactions appear in more
advanced stages than in the plastic-coated paperboard lam-
inate and tin containers, and the propagation or degrada-
tion stage of oxidation is observed. This takes place
simultaneously, due to the presence of oxygen that favours
the formation and decomposition of the hydroperoxides,
originating other volatile compounds with lower molecular
weights that are responsible for the disagreeable smell and
taste of the olive oil (Angerosa, Di Giacinto, & De Mattia,
1993; Solinas, Angerosa, & Cucurachi, 1985).
In the glass and plastic bottles, the action of light on the
olive oil is favouring photo-oxidation, although in both
containers, the pigments of the olive oil (chlorophylls and
pheophytins) have an oxidising eVect (Interesse et al., 1971;
Khan & Shadidi, 1999; Procida & Cichelli, 1999). In addi-
tion, the permeability to oxygen is an inXuence in the plas-
tic bottle, for which reason, at 6 months, the olive oil shows
a higher degree of oxidation and an increase in the peroxide
index is produced in all the samples.
The initial values of the coeYcients K270 and K232 are
between 0.15 and 0.17 for K270, and between 2.06 and 2.45
for K232, within the limits permitted by the legislation. In
Fig. 1 it can be seen that after 3 months of storage, primary
and secondary oxidation increases in all the samples. How-
ever, the olive oils stored in a plastic-coated paperboard
laminate and in tin containers show lower levels of absor-
bance at 270 nm than in the other containers and there is a
lesser degree of oxidation (primary and secondary) in the
plastic-coated paperboard laminate. After 6 months of
storage the increase of these coeYcients in all the samples
and in any type of container is conWrmed.
The lesser oxidative alteration in the containers stored in
the dark could be related to the antioxidant eVect of the nat-
ural pigments in the dark (Rahmani & Csallany, 1998), act-
ing synergistically with the phenols. But the opaque plastic
allows the entrance of oxygen and, once the irreversible
auto-oxidation reactions begin, they are forming hydroper-
oxides that simultaneously degrade other compounds.
An increase in oxidation also occurs in the samples stored
in glass and PET plastic containers, due to the increase in the
number of compounds resulting from the degradation of the
hydroperoxides, which is conWrmed by an increase of the
coeYcient K270 (Gasparoli, Taormina, & Fedeli, 1991; Olías-
Jiménez & Gutiérrez-González-Quijano, 1970). But, com-
pounds susceptible to primary oxidation are still found in
the samples, corroborated by the values of the coeYcient
524 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529

Plastic Opaque Glass Tin Tetra

Pl. plate Brik
4.000

3.000

K-232
2.000

1.000

0.000
0 3 6 3 6 3 6 3 6 3 6

Storage time (months)

A
A1 A2 A3 A4

Plastic Opaque Glass Tin Tetra

Pl. plate Brik
0.300

0.250
K-270

0.200

0.150

0.100
0 3 6 3 6 3 6 3 6 3 6

S torage time (months)

B
A1 A2 A3 A4

Fig. 1. Evolution of the absorption coeYcients K232 (A) and K270 (B) of extra-virgin olive oils during storage time and in diVerent containers.

K232, which increases in all the samples stored in glass and
plastic containers. Higher values of coeYcient K232 are found
in the olive oils stored in plastic bottles than in the rest of the
containers. This could be due to the joint action of light and
the permeability of this type of container to oxygen, which
catalyses the oxidation reaction. As a result the olive oil in
this type of container shows a higher oxidative rancidity
level after 3 months of storage. At the end of the period of
sample analysis, the number of characteristic compounds of
secondary oxidation continues to increase, with an evolution
in the diVerent types of container similar to that already
explained for up to 3 months of storage.
The initial content in humidity and volatile compounds
do not exceed the maximum value tolerated for extra-virgin
olive oil. Percentage of humidity increases with storage
time, above all in olive oils stored in normal and opaque
plastic bottles, followed by glass, tin, and plastic-coated
paperboard laminate. The least increase with respect to the
initial value is produced in this latter container (Table 2).
The evolution of this parameter is a danger for the conser-
vation of extra-virgin olive oil as this could acquire a
strange taste or smell and, moreover, other processes of
alteration could be induced in the product (Civantos, 1999).
In this sense, the olive oils stored in plastic bottles (normal
and opaque) are the ones that show a major variation and,
therefore, are the riskiest for conserving the quality of the
olive oil until it is consumed.
The percentage of impurities of all the initial samples is
below the level established by EEC Regulations. The evolu-
tion of this parameter in the diVerent containers is shown in
Table 2 and reXects an increase with storage time, although
to a diVerent degree according to the container used. In
normal and opaque plastic there is a greater increase of
impurities, duplicating in almost all the samples after 3
months of storage, followed by glass and tin containers.
The olive oil stored in a plastic-coated paperboard laminate
shows the least variation of this parameter. The degree in
which the impurities increase in each sample can be related
to the degree of oxidation. The olive oil stored in plastic
(normal and opaque) shows the highest level of rancidity,
followed by those stored in glass, tin and plastic-coated
paperboard laminate. As a consequence of oxidation, the
content in oxidised compounds, fatty acids, and impurities
increases, which result in a deterioration of the organoleptic
characteristics of the extra-virgin olive oil (Angerosa et al.,
1993).
Initially a markedly high content of phenols is found in
the extra-virgin olive oils (with the exception of A1 that
 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529 525

Table 2
Evolution of the humidity (%), impurity (%) and phenol content (ppm gallic acid) of extra-virgin olive oil during the storage time and in diVerent contain-
ers
Container Storage time (month) Extra-virgin olive oil samples
A1 § S.D.a A2 § S.D. A3 § S.D. A4 § S.D.
% Humidity
0 0.06 § 0.0001 0.07 § 0.0005 0.07 § 0.0004 0.07 § 0.0001
Plastic 3 0.07 § 0.0002 0.08 § 0.0003 0.08 § 0.0001 0.08 § 0.0001
6 0.09 § 0.0001 0.09 § 0.0005 0.09 § 0.0006 0.10 § 0.0005
Opaque plastic 3 0.07 § 0.0005 0.08 § 0.0001 0.07 § 0.0014 0.08 § 0.0006
6 0.09 § 0.0001 0.09 § 0.0001 0.09 § 0.0004 0.09 § 0.0001
Glass 3 0.07 § 0.0006 0.08 § 0.0005 0.07 § 0.0007 0.08 § 0.0008
6 0.08 § 0.0005 0.09 § 0.0006 0.08 § 0.0001 0.09 § 0.0004
Tin plate 3 0.07 § 0.0001 0.07 § 0.0001 0.07 § 0.0010 0.08 § 0.0004
6 0.08 § 0.0005 0.08 § 0.0001 0.08 § 0.0008 0.09 § 0.0001
Tetra-brik 3 0.07 § 0.0005 0.07 § 0.0009 0.07 § 0.0006 0.08 § 0.0004
6 0.08 § 0.0001 0.08 § 0.0001 0.08 § 0.0005 0.09 § 0.0006
% Impurity
0 0.017 § 0.0001 0.006 § 0.0003 0.005 § 0.0003 0.006 § 0.0001
Plastic 3 0.010 § 0.0002 0.010 § 0.0001 0.008 § 0.0003 0.013 § 0.0003
6 0.012 § 0.0001 0.013 § 0.0017 0.011 § 0.0004 0.019 § 0.0003
Opaque plastic 3 0.009 § 0.0003 0.009 § 0.0002 0.008 § 0.0002 0.012 § 0.0002
6 0.012 § 0.0003 0.011 § 0.0006 0.011 § 0.0001 0.018 § 0.0002
Glass 3 0.008 § 0.0001 0.008 § 0.0002 0.007 § 0.0002 0.010 § 0.0001
6 0.011 § 0.0001 0.010 § 0.0001 0.010 § 0.0001 0.015 § 0.0001
Tin plate 3 0.007 § 0.0001 0.008 § 0.0003 0.007 § 0.0001 0.009 § 0.0001
6 0.011 § 0.0001 0.010 § 0.0001 0.009 § 0.0003 0.015 § 0.0003
Tetra-brik 3 0.007 § 0.0001 0.007 § 0.0003 0.006 § 0.0004 0.008 § 0.0003
6 0.010 § 0.0001 0.009 § 0.0002 0.008 § 0.0001 0.014 § 0.0004
Phenol content (ppm gallic acid)
0 285 § 0.01 519 § 0.01 549 § 0.01 433 § 0.01
Plastic 3 160 § 0.01 360 § 0.05 451 § 0.06 303 § 0.01
6 39 § 0.01 120 § 0.04 139 § 0.01 108 § 0.06
Opaque plastic 3 164 § 0.01 387 § 0.01 466 § 0.01 305 § 0.01
6 49 § 0.04 176 § 0.01 210 § 0.07 113 § 0.01
Glass 3 172 § 0.01 429 § 0.01 475 § 0.01 310 § 0.01
6 66 § 0.01 194 § 0.07 217 § 0.01 165 § 0.05
Tin plate 3 175 § 0.01 476 § 0.00 477 § 0.01 320 § 0.01
6 70 § 0.01 241 § 0.05 250 § 0.01 172 § 0.00
Tetra-brik 3 176 § 0.01 489 § 0.01 478 § 0.01 324 § 0.01
6 74 § 0.01 267 § 0.03 265 § 0.05 173 § 0.01
a
S.D.: standard deviation of three replicates.

shows a content of 285 ppm, much lower than the other
olive oils) with values similar to those found by Vázquez,
del Valle, and del Valle (1976), Satue et al. (1995) and Bar-
ranco, Fernández-Escobar, and Rallo (1999). This high
concentration of phenols in the extra-virgin olive oils could
be related to the production process and its aptitude for
being consumed directly without the necessity of being pre-
viously reWned (GutWnger, 1981; Satue et al., 1995; Váz-
quez, Janer del Valle, & Janer del Valle, 1973). The lower
concentration in which it appears in sample A1 (Table 2)
could be due to the dependence of this parameter on diVer-
ent factors: agronomic (variety, cultivation system, envi-
ronmental factors, date of harvesting), extraction system
used (COI, 1987; Montedoro & Garofolo, 1984; Vázquez
et al., 1976), and inclusively could be related to the plastic
container used in the commercialisation of this particular
extra-virgin olive oil, as they are normally commercialised
stored in glass bottles.
These natural antioxidants provide the olive oil with cer-
tain characteristics at a chemical, organoleptic, and health
level. At a chemical level, there is a correlation between the
total polyphenols content and the stability of the olive oil
against oxidation (Monteleone, Caporale, Carlucci, &
Pagliarini, 1998; Tsimidou, Papadopaulos, & Boskou, 1992;
Vázquez et al., 1976). They are also related to the sensorial
characteristics of the virgin olive oil (COI, 1987). Thus, bit-
terness is considered to be a positive attribute in virgin olive
oil and is directly related to the content in polyphenols
(Jiménez et al., 1994; Uceda, Jiménez, Hermoso, & Frías,
1994).
There was a sharp decrease in phenol contents in all the
samples during storage, as a consequence of the hydrolysis
and oxidation of these compounds (Cinquanta, Esti, & La
Note, 1997), which involves a loss of stability and a deterio-
ration of the sensorial properties and, therefore, of the com-
mercial quality of the olive oil. The degradation of these
526 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529

Table 3
Evolution of the iodine index and saponiWcation index of extra-virgin olive oil during the storage time and in diVerent containers
Container Storage time (month) Extra-virgin olive oil samples
A1 § S.D.a A2 § S.D. A3 § S.D. A4 § S.D.
Iodine index (g I2/100 g oil)
0 82.41 § 0.14 84.89 § 0.03 85.69 § 0.31 87.93 § 0.02
Plastic 3 80.74 § 0.18 82.46 § 0.05 84.40 § 0.17 80.95 § 0.01
6 77.68 § 0.18 77.50 § 0.05 80.28 § 0.09 77.54 § 0.32
Opaque plastic 3 81.16 § 0.05 82.71 § 0.02 84.52 § 0.01 81.34 § 0.21
6 77.98 § 0.04 77.89 § 0.04 80.55 § 0.01 78.01 § 0.01
Glass 3 81.33 § 0.10 82.94 § 0.02 84.05 § 0.03 81.28 § 0.27
6 78.53 § 0.16 78.60 § 0.02 80.81 § 0.01 78.19 § 0.09
Tin plate 3 81.25 § 0.13 83.07 § 0.12 84.17 § 0.22 81.60 § 0.03
6 78.65 § 0.28 78.86 § 0.05 82.82 § 0.09 79.14 § 0.11
Tetra-brik 3 81.46 § 0.21 83.52 § 0.11 84.70 § 0.17 81.83 § 0.21
6 79.03 § 0.01 79.35 § 0.07 82.84 § 0.07 79.69 § 0.14
SaponiWcation index (mg KOH/g oil)
0 190.45 § 0.16 189.40 § 0.16 188.60 § 0.18 192.35 § 0.23
Plastic 3 188.20 § 0.10 187.10 § 0.03 186.59 § 0.01 190.71 § 0.14
6 185.13 § 0.11 181.40 § 0.03 183.49 § 0.23 186.00 § 0.10
Opaque plastic 3 188.49 § 0.44 186.73 § 0.05 186.39 § 0.40 191.07 § 0.01
6 185.80 § 0.06 182.28 § 0.01 184.39 § 0.01 187.00 § 0.01
Glass 3 188.59 § 0.23 188.34 § 0.25 186.97 § 0.14 190.48 § 0.25
6 185.75 § 0.12 183.45 § 0.12 184.65 § 0.10 187.22 § 0.30
Tin plate 3 188.73 § 0.12 187.29 § 0.10 185.45 § 0.27 191.17 § 0.35
6 185.65 § 0.01 183.70 § 0.11 184.52 § 0.01 187.42 § 0.01
Tetra-brik 3 189.19 § 0.28 187.53 § 0.23 185.72 § 0.01 191.40 § 0.28
6 187.11 § 0.11 184.46 § 0.28 185.01 § 0.01 187.56 § 0.11
a
S.D.: standard deviation of three replicates.

natural antioxidants is notable in the A1 sample of olive Plastic Opaque

80 Glass
oil; in which the initial concentration is reduced to one sev- Pl.
70
enth (284 to 38 ppm) after 6 months storage. 60 Tin Tetra
Colour index

The initial value of the iodine index of the samples is 50 plate Brik
very homogenous (Table 3), varying between 82.41 and 40 A1
87.93 g I2/100 g oil. After 3 months of storage a slight 30 A2
decrease is observed in a similar manner in all the contain- 20 A3
A4
ers tested. However, after 6 months of storage, the variation 10
of this parameter is conWrmed, not only with respect to the 0
0 3 6
temperature and storage time (TawWk & Huyghebaert, 3 6 3 6 3
1997), but also with respect to the type of container, show- 6 3 6
Storage time (month)
ing a sharper decrease with respect to the initial value in
plastic (normal and opaque), followed by glass and tin con- Fig. 2. Evolution of the colour index of extra-virgin olive oils during stor-
tainers. Plastic-coated paperboard laminate is again the age time and in diVerent containers.
container in which the extra-virgin olive oil is least aVected
by degradation of the double bonds that could be a conse- show levels that are within the limits established by EEC
quence of oxidation. Regulations.
The saponiWcation index of the samples at the beginning The colour index is identiWed using the A.B.T. scale of
of the investigation is within the range Wxed by EEC Regu- indexes (Fig. 2). After 3 months of storage there is no varia-
lations and the homogeneity of the results is noticeable, tion in colour. However, at the end of the investigation, a
showing values of between 188.60 and 192.35 mg KOH/g oil change was produced in the colour of the samples when plas-
(Table 3). After 3 months of storage a slight decrease of this tic or glass bottles had been used for storage, showing an
parameter is observed to a similar degree in the diVerent intensiWcation of the A.B.T. indexes and a brownish colour.
types of containers, which is conWrmed after 6 months in all This could be a consequence of the interaction of the natural
the containers. Although, in the olive oils stored in plastic pigments with the light, fundamentally the chlorophylls that
bottles (normal and opaque), the decrease is such that A2 degrade with photo-oxidation to produce pheophytins, and
and A3 show a saponiWcation index at the limit or below the appearance of other compounds resulting from advanced
the level permitted by the legislation. On the contrary, the oxidation (Kiritsakis, 1992; Mínguez, Rejano, Gandul, Sán-
samples stored in a plastic-coated paperboard laminate still chez, & Garrido, 1990). All these are produced to a greater
 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529 527

degree in the extra-virgin olive oil stored in plastic or glass 4. Conclusion

bottles than in plastic-coated paperboard laminate or tin con-
tainers (Olías-Jiménez & Gutiérrez-González-Quijano, 1971).
The modiWcation of the colour index means deterioration in
the organoleptic value of the extra-virgin olive oil (Garrido,
Gandul, Gallardo, & Mínguez, 1990) and a loss in the com-
mercial importance of the product, because it is one of the
sensorial parameters that make it attractive to the purchaser.
The initial content of fatty acids of all the samples is
within the established limits. The isomers that are detected in
extra-virgin olive oils are “cis” isomers, as the detection of
“trans” isomers would mean that the olive oil had been sub-
mitted to high pressures or temperatures (Civantos, 1999).
The high percentage of oleic acid is noticeable, which is the
predominant acid (Tables 4a and 4b). The analyses per-
formed after 3 months of storage show that the percentage
of fatty acids analysed has not varied with respect to the ini-
tial composition. Neither were signiWcant variations
observed after 6 months storage, although the fatty acids
margaric, margaroleic, and gadoleic were not detected,
despite minimal amounts (<0.30%) in the initial samples and
after 3 months of storage. A slight decrease in the percentage
of oleic acid is produced, which is supposed to be the conse-
quence of the degree of oxidation in the samples (Frega,
Mozzon, & Lercker, 1999). This was noted fundamentally in
the olive oils stored in plastic bottles (normal and opaque)
and above all in oil sample A1 with an initial content of
76.3% that fell to 73.3%. The percentage of polyunsaturated
fatty acids remains more or less constant throughout the
period of investigation.
The physical–chemical parameters analysed in the diVer-
ent samples of extra-virgin olive oil at the beginning of the
investigation are within the limits established by the legisla-
tion, but vary during the storage period and according to
the container employed. The principal cause of the deterio-
ration of the extra-virgin olive oil during storage is the oxi-
dation and hydrolysis reactions and the products resulting
from these, loss of natural antioxidants, variation in the
content of natural pigments – fundamentally chlorophylls
and carotenes – increase of rancidity, increase of impurities,
etc. This loss of extra-virgin olive oil quality is very more
marked the Wrst 3 months of storage, and afterwards
remained almost constant.
With respect to storage time, the acidiWcation and oxida-
tive rancidity of the olive oil increases during the storage
period. The degree of unsaturation tends to decrease as the
expiry date becomes closer and, although the percentage of
fatty acids remain constant until 3 months of storage, after
6 months an increase in the degree of saturation and a
decrease in the characteristic fatty acid (oleic) is observed as
a consequence of its oxidation. All of the physical–chemical
parameters analysed changed during 6 months resulting in
a deterioration in quality of this food product.
With respect to the type of container, it is seen that the
traditional container (plastic bottle) in which some extra-vir-
gin olive oils are packaged commercially is not the most ade-
quate for storage as, after 3 months, the oil has lost more
stability compared to the other containers as a consequence

Table 4a
Evolution of fatty acid content (% § S.D.a) of extra-virgin olive oil during the storage time and in diVerent containers
% Initial Plastic Opaque plastic Glass Tin plate Tetra-brik
0 month 3 months 6 months 3 months 6 months 3 months 6 months 3 months 6 months 3 months 6 months
A1 oil sample
Palmitic 10.3 § 0.1 10.6 § 0.7 10.6 § 0.2 10.3 § 0.1 10.6 § 0.3 10.5 § 0.3 10.7 § 0.2 10.3 § 0.1 10.5 § 0.1 10.5 § 0.1 10.7 § 0.1
Palmitoleic 0.8 § 0.0 0.8 § 0.1 0.9 § 0.1 0.8 § 0.1 0.9 § 0.1 0.8 § 0.1 0.8 § 0.1 0.8 § 0.1 0.9 § 0.1 0.9 § 0.1 0.9 § 0.1
Margaric 0.1 § 0.1 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.0 ND
Margaroleic 0.1 § 0.0 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.1 ND 0.1 § 0.0 ND 0.1 § 0.0 ND
Estearic 4.1 § 0.1 3.1 § 0.1 4.7 § 0.1 4.1 § 0.1 4.5 § 0.3 4.0 § 0.1 4.3 § 0.1 4.1 § 0.1 4.7 § 0.1 3.9 § 0.01 4.3 § 0.1
Oleic 76.3 § 0.1 75.3 § 0.1 73.3 § 0.4 76.5 § 0.1 73.5 § 0.1 76.0 § 0.1 75.1 § 0.1 76.6 § 0.1 75.0 § 0.1 76.0 § 0.2 75.4 § 0.1
Linoleic 5.0 § 0.1 6.2 § 0.1 6.5 § 0.4 5.0 § 0.1 6.5 § 0.1 5.0 § 0.0 3.7 § 0.1 4.9 § 0.0 5.2 § 0.1 5.0 § 0.1 5.4 § 0.2
Linolenic 0.7 § 0.1 0.6 § 0.0 0.8 § 0.1 0.7 § 0.0 0.7 § 0.2 0.7 § 0.1 0.7 § 0.1 0.6 § 0.1 0.6 § 0.1 0.7 § 0.1 0.7 § 0.1
Araquic 0.4 § 0.1 0.4 § 0.1 0.7 § 0.1 0.4 § 0.0 0.6 § 0.0 0.4 § 0.1 0.5 § 0.1 0.4 § 0.1 0.5 § 0.1 0.4 § 0.1 0.5 § 0.0
Gadoleic 0.2 § 0.1 0.2 § 0.1 ND 0.2 § 0.1 ND 0.2 § 0.0 ND 0.2 § 0.1 ND 0.2 § 0.1 ND
A2 oil sample
Palmitic 12.1 § 0.1 12.0 § 0.1 12.2 § 0.1 12.2 § 0.0 12.2 § 0.3 12.2 § 0.1 12.2 § 0.1 12.2 § 0.3 12.2 § 0.1 12.2 § 0.1 12.2 § 0.1
Palmitoleic 0.9 § 0.0 0.9 § 0.1 1.4 § 0.1 1.0 § 0.1 1.4 § 0.1 1.0 § 0.0 1.3 § 0.1 0.9 § 0.1 1.3 § 0.1 0.9 § 0.1 1.3 § 0.1
Margaric 0.1 § 0.1 0.1 § 0.0 ND 0.1 § 0.1 ND 0.1 § 0.0 ND 0.1 § 0.1 ND 0.1 § 0.0 ND
Margaroleic 0.2 § 0.1 0.2 § 0.1 ND 0.2 § 0.1 ND 0.2 § 0.1 ND 0.2 § 0.1 ND 0.2 § 0.1 ND
Estearic 2.9 § 0.0 3.0 § 0.1 3.7 § 0.3 2.9 § 0.1 3.8 § 0.1 3.0 § 0.1 3.7 § 0.1 2.9 § 0.1 3.5 § 0.1 2.9 § 0.1 3.5 § 0.3
Oleic 72.4 § 0.1 72.3 § 0.1 70.5 § 0.3 72.2 § 0.1 70.8 § 0.1 72.4 § 0.1 71.0 § 0.1 72.3 § 0.2 71.4 § 0.1 72.3 § 0.1 71.5 § 0.2
Linoleic 7.9 § 0.0 7.9 § 0.1 7.9 § 0.1 7.9 § 0.1 7.9 § 0.1 7.8 § 0.0 7.9 § 0.0 7.8 § 0.1 7.8 § 0.1 7.8 § 0.2 7.9 § 0.1
Linolenic 0.7 § 0.1 0.7 § 0.0 0.8 § 0.1 0.6 § 0.0 0.8 § 0.1 0.6 § 0.0 0.8 § 0.1 0.6 § 0.0 0.8 § 0.1 0.6 § 0.0 0.7 § 0.1
Araquic 0.4 § 0.1 0.4 § 0.1 0.6 § 0.1 0.4 § 0.1 0.6 § 0.1 0.4 § 0.1 0.5 § 0.1 0.4 § 0.0 0.5 § 0.0 0.4 § 0.1 0.5 § 0.1
Gadoleic 0.3 § 0.1 0.3 § 0.0 ND 0.3 § 0.1 ND 0.3 § 0.0 ND 0.3 § 0.0 ND 0.3 § 0.0 ND
ND: not detected.
a
S.D.: standard deviation of three replicates.
528 A.I. Méndez, E. Falqué / Food Control 18 (2007) 521–529

Table 4b
Evolution of fatty acid content (% § S.D.a) of extra-virgin olive oil during the storage time and in diVerent containers
% Initial Plastic Opaque plastic Glass Tin plate Tetra-brik
0 month 3 months 6 months 3 months 6 months 3 months 6 months 3 months 6 months 3 months 6 months
A3 oil sample
Palmitic 11.9 § 0.1 11.8 § 0.1 11.8 § 0.1 11.7 § 0.1 11.7 § 0.1 12.1 § 0.1 11.7 § 0.4 11.8 § 0.1 11.8 § 0.2 11.7 § 0.1 11.6 § 0.0
Palmitoleic 0.9 § 0.1 0.9 § 0.1 1.1 § 0.1 0.9 § 0.1 1.1§ 0.1 0.9 § 0.1 1.0 § 0.1 0.9 § 0.1 1.1 § 0.1 1.0 § 0.0 1.0 § 0.1
Margaric 0.1 § 0.1 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.1 ND 0.1 § 0.0 ND 0.1§ 0.0 ND
Margaroleic 0.2 § 0.1 0.2 § 0.0 ND 0.2 § 0.0 ND 0.2 § 0.1 ND 0.2 § 0.1 ND 0.2 § 0.0 ND
Estearic 3.1 § 0.0 3.0 § 0.1 3.9 § 0.1 3.1 § 0.1 3.7 § 0.1 3.0 § 0.0 3.6 § 0.4 3.1 § 0.1 3.3 § 0.2 3.1 § 0.0 3.2 § 0.0
Oleic 72.8 § 0.1 72.8 § 0.1 71.8 § 0.1 73.1 § 0.1 72.4 § 0.4 72.6 § 0.1 72.3 § 0.4 73.0 § 0.2 72.5 § 0.2 73.1 § 0.1 73.0 § 0.1
Linoleic 7.6 § 0.1 7.6 § 0.0 7.7 § 0.1 7.6 § 0.1 7.7 § 0.1 7.5 § 0.1 7.6 § 0.0 7.6 § 0.1 7.7 § 0.1 7.6 § 0.1 7.6 § 0.1
Linolenic 0.7 § 0.1 0.7 § 0.0 0.7 § 0.1 0.7 § 0.0 0.7 § 0.1 0.7 § 0.0 0.7 § 0.0 0.7 § 0.0 0.7 § 0.1 0.7 § 0.0 0.7 § 0.1
Araquic 0.4 § 0.1 0.4 § 0.0 0.6 § 0.1 0.4 § 0.0 0.6 § 0.1 0.4 § 0.0 0.5 § 0.1 0.4 § 0.1 0.5 § 0.1 0.4 § 0.1 0.5 § 0.1
Gadoleic 0.2 § 0.0 0.3 § 0.1 ND 0.3 § 0.0 ND 0.3 § 0.1 ND 0.3 § 0.1 ND 0.3 § 0.1 ND
A4 oil sample
Palmitic 10.8 § 0.2 10.5 § 0.2 10.7 § 0.0 10.6 § 0.1 10.7 § 0.1 10.6 § 0.1 10.7 § 0.1 10.5 § 0.1 10.6 § 0.1 10.8 § 0.2 10.6 § 0.1
Palmitoleic 0.8 § 0.1 0.7 § 0.1 0.9 § 0.1 0.8 § 0.1 0.9 § 0.1 0.8 § 0.1 0.9 § 0.1 0.7 § 0.1 0.9 § 0.1 0.8 § 0.1 0.9 § 0.1
Margaric 0.1 § 0.0 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.0 ND 0.1 § 0.1 ND
Margaroleic 0.1 § 0.0 0.1 § 0.1 ND 0.1 § 0.1 ND 0.1 § 0.1 ND 0.1 § 0.1 ND 0.1 § 0.0 ND
Estearic 3.3 § 0.1 3.3 § 0.1 3.8 § 0.1 3.3 § 0.1 3.7 § 0.1 3.6 § 0.1 3.6 § 0.1 3.3 § 0.1 3.5 § 0.1 3.3 § 0.1 3.5 § 0.1
Oleic 77.5 § 0.2 77.6 § 0.4 76.2 § 0.1 77.7 § 0.3 76.5 § 0.2 77.4 § 0.3 77.0 § 0.1 77.7 § 0.2 77.4 § 0.1 77.7 § 0.2 77.3 § 0.2
Linoleic 4.2 § 0.1 4.2 § 0.1 4.4 § 0.1 4.2 § 0.1 4.4 § 0.1 4.1 § 0.1 4.3 § 0.1 4.1 § 0.1 4.2 § 0.0 4.1 § 0.1 4.3 § 0.0
Linolenic 0.7 § 0.0 0.6 § 0.1 0.7 § 0.1 0.7 § 0.1 0.7 § 0.1 0.7 § 0.0 0.7 § 0.1 0.6 § 0.0 0.7 § 0.1 0.6 § 0.1 0.7 § 0.1
Araquic 0.4 § 0.1 0.4 § 0.1 0.6 § 0.1 0.4 § 0.1 0.6 § 0.1 0.5 § 0.0 0.6 § 0.1 0.4 § 0.1 0.5 § 0.1 0.4 § 0.1 0.4 § 0.1
Gadoleic 0.2 § 0.0 0.2 § 0.0 ND 0.2 § 0.1 ND 0.3 § 0.0 ND 0.2 § 0.1 ND 0.2 § 0.0 ND
ND: not detected.
a
S.D.: standard deviation of three replicates.

of the action of oxygen and light that induce a rapid deterio-
ration in plastic bottles. Likewise, acidiWcation, an increase in
impurities, loss of the phenolic fraction, etc. is favoured. The
storage of extra-virgin olive oil in plastic bottles, but isolated
from light (covered with aluminium foil), allows the conser-
vation of its properties for longer than in the traditional
plastic bottle, which suggested that the light transmission on
the PET bottle, during this initial storage time, is unimpor-
tant compared to oxygen permeability. Although after 6
months of storage deterioration is similar, due to its perme-
ability to oxygen.
Glass acts as a barrier to oxygen, which cannot pass
through it, avoiding the loss of certain components that
deteriorate in its presence, but it does allow the direct
action of light on the olive oil, producing oxidative rancid-
ity even earlier than in the opaque plastic container, as a
consequence of its sensibility to photo-oxidation. Although
most of the extra-virgin olive oils are packaged commer-
cially in glass bottles as an indicator of high quality, this
container does not maintain throughout its commercial life,
the sensorial and nutritive attributes for which the product
is so much appreciated.
The plastic-coated paperboard laminate and tin contain-
ers are possibly the least used commercially at the present
time. However, they would be the most appropriate for
maintaining the quality of extra-virgin olive oil, at least
during 6 months. Both, in common, protect against light
and gases, but the Tetra-brik Aseptic® conserves the initial
characteristics of the product much better than any of the
containers.
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