J Am Oil Chem Soc (2012) 89:577583

DOI 10.1007/s11746-011-1958-x

ORIGINAL PAPER

Accelerated Shelf Life Testing (ASLT) of Oils by Light

and Temperature Exploitation
Lara Manzocco Agnese Panozzo Sonia Calligaris

Received: 16 March 2011 / Revised: 20 July 2011 / Accepted: 7 October 2011 / Published online: 27 October 2011
AOCS 2011

Abstract The peroxide formation rate was measured in

sunflower and soybean oils exposed to increasing light
intensity, from 0 to 8000 lx, at 10, 20 and 30 C. Results
indicated that shelf life estimation of photosensitive foods
under actual or accelerated conditions cannot be correctly
achieved if the effect of light is not taken into account. At
each lighting level, the Arrhenius equation was applied to
develop a model predicting oil shelf life. Thermal activation energy was lower than 50 kJ/mol, indicating temperature to be a scarcely efficient accelerating factor. In
contrast, the oxidation rate was significantly affected by
light according to a power law equation, whose parameters
describe the electromagnetic activation energy of the
reaction. The model accounting for the effect of light on
oxidation rate was merged with the Arrhenius equation
to get a model predicting shelf life on the basis of the
concomitant changes in both temperature and light.
Keywords Oxidation  ASLT  Light  Temperature 
Sunflower oil  Soybean oil

Introduction
In order to reduce the time needed to obtain shelf life data,
quality depletion kinetics is customary accelerated by
increasing the storage temperature [1]. This procedure is
widely accepted since temperature can be easily modified
and controlled during the tests but also because the temperature dependence of quality depletion can be modeled
L. Manzocco (&)  A. Panozzo  S. Calligaris
Dipartimento di Scienze degli Alimenti, Universita` di Udine,
via Sondrio 2/A, 33100 Udine, Italy
e-mail: lara.manzocco@uniud.it

by the simple and remarkably accurate Arrhenius equation.

Unfortunately, not all quality depletion phenomena are
similarly accelerated by the increase in temperature.
They are actually characterized by different magnitudes
of apparent activation energy going from 25 up to
300400 kJ/mol [24]. When the thermal activation energy
is low, the increase in temperature does not promote any
significant acceleration in the rate of the alterative phenomena. This means that the time saved when performing
accelerated shelf life testing (ASLT) by increasing temperature may be small or even negligible.
Low activation energy, and thus scarce temperature
dependence, are often associated with light induced oxidation of foods containing lipids, vitamins, pigments and/
or flavors [57]. In this regard, it is noteworthy that many
foods are packed in see-through materials and displayed on
highly lit shelves (600800 lx) in order to attract consumers [8]. This is a common practice even for photosensitive products such as, among others, oils, beer, soft drinks
and chips. Although light exposure is well known to cause
intense quality depletion [9], shelf life testing of photosensitive foods is generally carried out for assessing quality
changes during storage while controlling the sole temperature ignoring the effect of light. Such an approach may be
tricky since it could lead to a dangerous overestimation of
product shelf life.
The shelf life testing of light-sensitive food should take
into proper account the effect of light on alterative reaction
kinetics by simulation of real storage conditions or by
exploiting light as an alternative environmental acceleration factor in ASLT. In the case of fat and oils, the AOCS
light stability method [10] defines a protocol to assess the
light sensitivity of oils. In particular, it is recommended to
expose samples to high light intensity levels from 4,200 to
7,500 lx. These conditions are definitely far from those

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actually experienced by the product on the shelves. For

this reason, the AOCS method cannot be considered as
an accelerated shelf life test since it does not allow the
behavior of samples under actual storage conditions to be
evaluated. The only way to exploit light as an acceleration
factor for shelf life prediction is the availability of models
describing the effect of light on quality depletion kinetics.
Until now, little effort has been made to rationalize the use
of this environmental variable and integrate its effect into
the generally accepted shelf life prediction models. In
addition, there is little information about how to elaborate
data relevant to shelf life tests performed under light. This
is probably attributable to unavailability of robust, validated and generally accepted mathematical models correctly predicting the effect of light on quality depletion. If
these models were available, they should combine the
effect of both light and temperature to obtain an integrated
shelf life model.
This investigation was designed to attempt to fill this
gap. To this aim, the effect of widely different levels of
light and temperature on the oxidation rate was investigated. Sunflower and soybean oils, which are often packed
in transparent materials and exposed on retail shelves to
intense fluorescent light, were taken as typical examples of
light sensitive products. Rates of peroxide formation during
storage were used to develop models predicting the oil
shelf life as a function of: (1) temperature (2) light and (3)
concomitant changes for both factors. The model was
validated and the choice of temperature or light to perform
ASLT was discussed in terms of time saved to get an
accurate shelf life value.

J Am Oil Chem Soc (2012) 89:577583

Fig. 1 Schematic representation of the experimental setup during

ASLT

between 250 and 780 nm. Oil samples were stored for up to
8 weeks at 10, 20 or 30 C under different lighting levels
from 0 to 8000 lx.
Analytical Determinations

Materials and Methods

Temperature

Materials

The sample temperatures were measured (with an accuracy

of 0.2 C) by a copper/constantan thermocouple probe
(type T thin thermocouple, Ellab, Denmark).

Commercial sunflower and soybean oils were purchased

from a local supermarket. Aliquots of 3 g of oil were
introduced into 10 mL capacity clear glass vials and hermetically sealed with butyl septa and metallic caps with air
in the headspace (Carlo Erba, Milano, Italy). The liquid
headspace volume ratio was 1:2. The vials were stored in
an incubator (Climacell 222, MMM Medcenter, Einrichtungen GmbH, Graefling, Germany) at different distances
from the fluorescent tubes positioned vertically in the
internal part of the door of the incubator (Fig. 1). No
temperature changes were observed as a consequence of
lighting. A control sample was stored inside the incubator
in a black box (dark conditions). Fluorescent tubes SLI
Activa-172 (34.2 W, Sylvania, SLI Lighting, Raunheim,
Germany) were used. Irradiance of the fluorescent tubes
was 1.199 mW/cm2 and their emission spectrum was

123

Illuminance
The lighting level was measured using a portable luminometer (HD-2102.2 Delta Ohm, Padova, Italy).
Peroxide Value
The peroxide value assessment was carried out according
to the European Official Methods of Analysis [11].
Oxidation Rate
Apparent zero order rate constants of peroxide formation
(k) were calculated by linear regression of at least five

579

Data Analysis
The results reported in this work are the average of at least
three determinations and the coefficients of variation, calculated as the percentage ratio between the standard deviation and the mean value, were less than 5% for peroxide
value and peroxide formation rate. Regression analysis by
least squares regression was performed by Table-curve 2D
(version 5.0, Systat Software Inc., Richmond, CA) and the
goodness of fitting evaluated on the basis of statistical
parameters of fitting (R2, p, SE). To make a better estimate
of the apparent activation energy and pre-exponential factor, the effect of temperature on the rate of lipid oxidation
was evaluated by means of the reparameterized Arrhenius
equation:


k kref  e

ERa

1
1
T Tref

40
35

b
Peroxide value (meq O 2/kgoil )

points from the initial part of the curves excluding the lag
phase, when present.

Peroxide value (meq O 2 /kgoil )

J Am Oil Chem Soc (2012) 89:577583

8000 lx
5300 lx
2700 lx
2000 lx
1400 lx
600 lx
0 lx

30
25
20
15
10
5
0
0

40
35
30
25
20
15
10
5
0

where R is the molar gas constant (8.31 J/K mol), T is the

absolute temperature (K); Ea is the thermal activation
energy (J/mol) and kref is oxidation rate (meq O2/kgoil/days)
at a reference temperature (Tref) chosen in the middle of the
temperature range considered in the experimental plan. As
reference temperature it was used 293.15 K (20 C).

Results and Discussion

Sunflower and soybean oils were exposed to increasing light
intensity at 20 C. During storage, samples were analyzed
for their peroxide value (Fig. 2). Oils stored under dark
presented a typical lag phase (17 and 46 days respectively for
sunflower and soybean oils) followed by a slow increase in
peroxide value which did not exceed 10 meq O2/kgoil after
8 weeks (data not shown). By contrast, no lag phase was
detected in samples stored under light which show peroxide
values quickly increasing within few days. In addition, for
both oils, the enhancement in peroxide value during storage
was higher as light intensity increased. These results are in
agreement with a number of literature indications demonstrating the catalytic effect of light on lipid oxidation [12].
It is noteworthy that oils are generally exposed on the
retail shelves under light intensities from 500 to 1,000 lx
[8]. Based on the dramatic effect of light exposure on oil
oxidation (Fig. 2), it is evident that performing accelerated
shelf life testing (ASLT) by taking into account the sole
storage temperature and neglecting the role of light could
lead to dangerous underestimation of shelf life.
In order to understand the relative importance of light
and temperature on oil oxidation, additional experiments

Time (days)

Fig. 2 Peroxide value of sunflower (a) and soybean (b) oils during
exposure to increasing light intensity at 20 C. Bars represent
standard error of peroxide value

were performed by storing samples under increasing light

intensity but at different temperatures (i.e. 10 and 30 C).
As expected, peroxide value was found to increase
according to the same evolution observed in Fig. 2, even if
to a lower or higher extent depending on storage temperature (data not shown). The pseudo zero order rate constants (k) of peroxide formation were calculated by linear
regression of at least five points from the initial part of the
curves, excluding the lag phase when present. In all cases,
determination coefficients (R2) resulted higher than 0.95.
The zero order kinetics has been previously applied by
different Authors to describe the peroxide formation
changes during storage [1315].
It can be inferred that both temperature and light are
potentially exploitable as accelerating factors to perform
ASLT of light-sensitive food, such as vegetable oils. Rate
constants of peroxide formation were thus elaborated to
develop mathematical models predicting the oil shelf life as
a function of: (1) temperature (2) light and (3) concomitant
changes in both factors. For clarity purpose, the modeling
procedures will be discussed separately.
Temperature as an Accelerating Factor
The applicability of the Arrhenius model, which is conventionally used to describe the effect of temperature on

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J Am Oil Chem Soc (2012) 89:577583

Ln k (meq O 2/kgoil /days)

reaction rates [1], was evaluated with reference to the

development of ASLT of sunflower and soybean oils
(Fig. 3). Data were elaborated according to the reparameterized Arrhenius model (Eq. 1) to compute the values of
activation energy (Ea) and oxidation rate at the reference
temperature of 20 C (kref). Table 1 shows the results of
this analysis. The model allowed the effect of temperature
on oil oxidation at all light intensities considered to be
described well. Ea values resulted consistent with those
typically reported in the literature for lipid oxidation [16,
17]. In addition, in the dark, the temperature dependence of
sunflower oil was significantly higher than that observed in
soybean oil. The intensity of light strongly affected the
temperature dependence of oil oxidation and this effect
varied with the lipid matrix considered. The activation
energy of sunflower oil oxidation was within 23 and 36 kJ/
mol for all samples stored under light. The higher the
intensity of the light, the higher was the temperature
dependence of k. In the case of soybean oil, a marked
increase in Ea values was detected only for light intensities
exceeding 2,700 lx. It is noteworthy that, at 5,300 and
8,000 lx, kref values were significantly higher for soybean
oil as compared to the sunflower one. This result indicates
that soybean oil oxidation is much more light sensitive than
sunflower oil.

5300 lx
1
2700 lx
0

Ln k (meq O 2/kgoil /days )

0.0033

0.0034

0.0035

0.0036

8000 lx
5300 lx
2700 lx
2000 lx

1400 lx
0

600 lx
0 lx

-1

0.0033

0.0034

0.0035

0.0036

Temperature (1/K)

Fig. 3 Arrhenius plot of pseudo zero order oxidation rate constant

(k) of sunflower (a) and soybean (b) oils exposed to increasing light
intensity. Points are experimental data. Lines are results of best fitting
analysis according to Eq. 1

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PVlim  PVo


1
EaR T1 Tref
kref  e

where SLL,T is the shelf life of the oil stored at a given

light intensity (L) and temperature (T), PVo is the peroxide
value at time zero and PVlim is the peroxide value corresponding to the acceptability limit. Since for seed oils,
there are no regulatory indications defining the acceptability limit available, the food industry operators have to
arbitrarily choose the PVlim value defining the end of shelf
life [18]. It is noteworthy that the time saved when performing the shelf life test under temperature accelerated
conditions may be considerably different, depending on
the values of Ea. For instance, oxidation of soybean oil
stored at 600 lx, thus simulating conventional lightning on
retail shelves, shows an Ea value around 30 kJ/mol. This
means that an increase in 10 C during the ASLT would
allow the testing time to be reduced by circa 20%. In order
to make oxidation quicker, thus reducing considerably the
testing time, the temperature of the test should be largely
increased. However, as reported in the literature [12, 19,
20], this approach is frown with the risk of excessive
rancidity level. It is evident that there is no reason to
perform an accelerated shelf life test if it does not provide
a significant advantage in terms of time saved. In other
words, for such products, performing an ASLT based on
temperature increase would be of limited help in order to
save time.
Light as an Accelerating Factor

0 lx

-2
0.0032

SLL;T

1000 lx

-1
-2
0.0032

-1

8000 lx

By keeping constant the level of lightning, it is thus

possible to perform ASLT of oils exploiting the accelerating effect of temperature, as described by the SL equation
based on the pseudo zero order:

Observing Fig. 1, it is clear that besides the temperature,

light intensity could also be effectively used as an accelerating factor in ASLT of photosensitive foods, such as
vegetable oils. To this regard, it is interesting to note that
the magnitude of light and temperature effects on oxidation
rate is considerably different (Fig. 3). In fact, in the dark,
the oxidation rate was always very slow independent of
storage temperature. By contrast, a slight increase in light
intensity was associated to a remarkable enhancement in
oxidation rate. Similarly to ASLT based on temperature,
data relevant to oxidation rate under increasing lightning
conditions could be elaborated to extrapolate the rate at
milder conditions usually experienced by the product on
the retail shelves. In order to develop a mathematical
model to correctly predict the effect of this accelerating
factor on the oxidation rate, k values were plotted as a
function of light intensity and submitted to best fitting

J Am Oil Chem Soc (2012) 89:577583

Table 1 Results of regression
analysis according to the
Arrhenius equation of pseudo
zero order oxidation rate
constant of sunflower and
soybean oils exposed to
increasing light intensity

581

Light intensity (lx)

Sunflower oil

Soybean oil

0.80

0.99

0.55

23.35

7.45

0.97

0.51

2,700

33.42

8.93

0.96

0.85

5,300

34.01

12.30

0.99

0.34

8,000

36.26

14.50

0.99

0.30
0.27

21.88

0.71

0.99

600

29.99

2.77

0.97

0.58

1,400

25.14

6.01

0.99

0.01

2,000

19.05

7.62

0.78

1.20

2,700

25.39

11.21

0.99

0.08

5,300

39.08

17.44

0.99

0.06

8,000

42.38

21.95

0.99

0.16

k (meq O 2 /kgoil/days)

30
30 C

20
20 C
10 C

5
0
0

2000

4000

6000

k (meq O2 /kgoil/days)

8000

45
30 C

40
35
30
25

20 C

20
15

10 C

10
5
0
0

2000

4000

6000

8000

Light intensity (lx)

Fig. 4 Pseudo zero rate constants (k) of peroxide formation of

sunflower (a) and soybean (b) oils as a function of light intensity
during storage at 10, 20 and 30 C. Points are experimental data.
Lines are results of best fitting analysis according to Eq. 3

(Fig. 4). The data turns out to be well described by a power

law equation:
k kd El1  LEl2

SE

64.76

35

10

R2

40

15

-1
kref (meq O2 kg-1
oil days )

1,000

45

25

Ea (kJ/mol)

where L is light intensity (lx), kd is the estimated value of

the reaction rate under dark and El1 and El2 are the
experimental parameters of the model, namely the electromagnetic energy required to activate the reaction.
Table 2 shows the values of kd, El1 and El2 estimated by
best fitting as well as relevant statistical parameters. El1 and

El2 parameters, reported in Table 3, describe the light

dependence of the oil oxidation rate. Similarly to the
thermal activation energy (Ea), they account for the electromagnetic energy required to activate the oxidative
reaction. It is worth mentioning that two parameters
(El1 and El2 ) are required to accurately describe the light
dependence of the reaction. Indeed they are also inversely
correlated (r [ 0.97). From a mathematical point of view,
El1 accounts for the initial curvature of the function (Eq. 3),
which can be visually appreciated at light intensity lower
than circa 3,000 lx. Similarly, El2 particularly contributes
to the effect of light at higher lighting conditions. For
instance, at each temperature, the El1 parameters are higher
in sunflower oil than in soybean oil (Table 3). Conversely,
El2 parameters assume values lower in sunflower oil as
compared to soybean oil. This means that sunflower oil
oxidation is strongly light dependent at low light intensity
while this dependence decreases under intense lightning.
This effect is clearly evident when examining the evolution
of data shown in Fig. 4.
By keeping a constant temperature during the test, it is
thus possible to perform ASLT of oil oxidation exploiting
the accelerating effect of light as described by the SL
equation based on the pseudo zero order:
SLL;T

PVlim  PVo
kd El1  LEl2

Equation 4 is actually a model allowing the prediction

of oil shelf life to be made by changing the light intensity at
a given temperature T. The only independent variables of
the model are light intensity (L), which is the enlighten
conditions experienced by the oil on the retail shelves, and
the acceptability peroxide value limit (PVlim). Kd, El1 and
El2 are intrinsic properties of the oil and depend on its
composition.
Similarly to ASLT based on temperature, in the case of
the exploitation of light, the time saved when performing

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J Am Oil Chem Soc (2012) 89:577583

Table 2 Best fitting parameters, determination coefficient (R2) and

fitting standard error (SE) according to Eq. 3 for sunflower and soybean oils stored at 10, 20 and 30 C under increasing light intensity
Temperature ( C)

Sunflower oil

20

30

kd

0.312

0.718

1.978

El1

0.964

0.570

0.154

El2

0.235

0.350

0.552

R
Soybean oil

10

0.98

0.99

0.99

SE

0.657

0.265

0.460

kd
El1

0.485
0.054

0.641
0.019

0.910
0.010

El2

0.602

0.783

0.923

0.98

0.99

0.99

0.627

0.821

0.776

SE

Table 3 Best fitting parameters, determination coefficient (R2) and

fitting standard error (SE) according to Eq. 5 for sunflower and soybean oils stored at 10, 20 and 30 C under increasing light intensity
Light dependence parameter
El1

El2

Sunflower oil

Soybean oil

m1

-0.040

-0.002

q1

12.444

0.669

R2
SE

0.99
0.009

0.90
0.010

m2

0.016

0.016

q2

-4.272

-3.945

R2

0.98

0.99

SE

0.035

0.017

the shelf life test under light accelerated conditions

depends on the values of El1 and El2 . For instance, the
percentage of time which is saved when the light intensity
during the life test is increased by 1,000 lx approaches
about 80% for both soybean and sunflower oil. This result
allows to clearly state that light can be a very efficient
accelerating factor in shelf life studies.
Temperature and Light as Accelerating Factors
The effect of temperature on the light dependence of oxidation rate in sunflower and soybean oils was evaluated by
plotting the values of kd, El1 and El2 as a function of
temperature (data not shown). Being kd the rate of oxidation under dark, they were plotted according to the
Arrhenius model (Eq.1) thus giving values of Ea and kdref
equal to those reported in Table 1 for oils stored in the dark
(L = 0 lx). By best fitting analysis it was possible to find
the model describing the temperature dependence of the
parameters El1 and El2 . They turned out to be well described by the simple equation of a straight line:

123

El m  T q

where El is the light activation parameter at low (El1 ) or

high (El2 ) light intensity and m and q are the experimental
regression parameters. This equation actually describes the
effect of temperature on light activation parameters when
the oil is stored under illumination.
Table 3 shows the values of the parameters of Eq. 5
with relevant determination coefficients (R2) and fitting
standard errors (SE) for sunflower and soybean oil. Based
on these considerations, it is useful to integrate into a single
model the effect of both variables, light and temperature.
Thus, the Arrhenius model (Eq. 1) and Eq. 5 were substituted into the power law equation (Eq. 3):


k kdref  e

Ea

1
1
T Tref

m1  T q1 Lm2 Tq2

Such a model is particularly useful and versatile since it

allows the prediction of the oxidation rate under different
experimental conditions. In fact, if the oil is stored in the
dark (L = 0 lx) at increasing temperatures, the model is
brought back to the Arrhenius equation. In contrast, if the
oil is stored at room temperature under increasing light
intensity, the model returns to Eq. 3. Finally, Eq. 6 allows
the prediction of the oxidation rate at any combination of
temperature and light intensity within the experimental
range considered.
In order to verify the reliability of the model proposed, a
full validation test on external data was carried out considering different temperature and light conditions. In particular, sunflower and soybean oils stored at 10, 25 and
30 C under different light conditions were considered. The
k values were predicted by substituting light and temperature data in Eq. 6. Predicted k values were compared with
those experimentally assessed (Fig. 5). It can be observed
that the proposed model allowed a very good prediction of
the oxidation rate in both sunflower and soybean oil. In fact,
regression analysis carried out between experimental and
predicted data pointed out a very low standard error (0.05)
and a determination coefficient (R2) close to 1 (p \ 0.05).
In order to achieve a shelf life model accounting for
both light and temperature on oil oxidation, Eq. 6 was
substituted in Eq. 4. The general shelf life model results as
follows:
SL
kdref  e

Ea

PVlim  PVo


1
1
T Tref

m1  T q1 Lm2 Tq2

When both temperature and light intensity are used to

accelerate oxidation, they exert a synergistic acceleration
effect which allows the prediction time to be dramatically
reduced. For instance, an accurate estimation of the shelf life
of soybean oil at 20 C under 600 lx light intensity would
take circa 23 weeks, whilst performing the test at 30 C

J Am Oil Chem Soc (2012) 89:577583

583

References

Predicted k (meq O2/kgoil/days)

30
25C, 8000 lx

25 C, 8000 lx

25

25 C, 5300 lx
20
25 C, 2700 lx

15

25 C, 2700 lx

30 C, 800 lx

10

25 C,1000 lx
Soybean oil

30 C, 800 lx
10 C, 800 lx
10 C, 800 lx

0
0

25 C 0 lx
5

10

Sunflower oil

15

20

25

30

Experimental k (meq O2/kgoil/days)

Fig. 5 Pseudo zero order oxidation rates (k) predicted by Eq. 6 as a

function of experimental oxidation rate of sunflower and soybean oils
stored at 10, 25 and 30 C under different lightning conditions

under 5,000 lx the same result could be achieved in less than

2 days. It should be noted that the final shelf life value
obtained from the application of such predictive model
could have a wide confidence interval due to the different
sources of uncertainty coming from the use of multiple fitted
constants. Although this procedure is affected by the risk of
a certain level of uncertainty, it could represent a rational
compromise between the contrasting requirements of
estimating shelf life with adequate accuracy but in
reasonable times and with sustainable costs.
Even if the developed model is valid for sunflower and
soybean oils in the specific light and temperature range
considered in this study, the proposed approach could be
used to set up shelf life predictive models for other types of
light sensitive products.

Conclusion
An adequate accelerating factor should be able to significantly decrease the time required for the test. Depending on
the reaction sensitivity to temperature and light, the most
appropriate accelerating factor should be exploited to
perform accelerated shelf life testing. In this context, the
analysis of the magnitude of thermal (Ea) and electromagnetic (El1 and El2 ) activation energy could represent a
valid tool to support the operator in selecting the most
efficient accelerating factor. The specific application presented in this paper was relevant to vegetable oils, but the
suggested procedure can be definitely extended to other
photosensitive foods. This is certainly an open research
field which will require more attention from food scientists
and researchers in the future.

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