Hindawi

Journal of Food Quality

Volume 2018, Article ID 1639260, 15 pages
https://doi.org/10.1155/2018/1639260

Review Article
Shelf Life of Extra Virgin Olive Oil and Its Prediction Models

1 1,2
Xueqi Li and Selina C. Wang
1
University of California Davis Olive Center, Davis, CA 95616, USA
2
Department of Food Science and Technology, University of California, Davis, Davis, CA 95616, USA

Correspondence should be addressed to Selina C. Wang; scwang@ucdavis.edu

Received 26 October 2017; Accepted 2 January 2018; Published 31 January 2018

Academic Editor: Amani Taamalli

Copyright © 2018 Xueqi Li and Selina C. Wang. This is an open access article distributed under the Creative Commons Attribution
License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly
cited.

Extra virgin olive oil (EVOO), with high unsaturation degree (oleic acid, linoleic acid, and linolenic acid), is prone to oxidation
during production and storage even with the presence of abundant antioxidants (e.g., phenolic compounds, alpha-tocopherol, and
chlorophyll). The level of oxidation degradation is greatly affected by the EVOO chemical composition (free fatty acids, saturated
and unsaturated fat ratio, total phenol content, etc.) and storage conditions (packaging material, oxygen, temperature, and light).
With the increasing demand on qualitative acceptability and food safety of an EVOO product, consumers rely heavily on “shelf life”
as a good indicator. Hence, it is critical for olive oil producers to provide accurate and practical information on shelf-life prediction.
This review analyzes ten shelf-life prediction models that used various parameters and approaches for model establishment. Due to
the complexity of chemical interactions between oil phase and environment under real-time storage and rapid accelerated testing
conditions, further investigation is needed to scrutinize and minimize the discrepancies between real-time shelf life and predicted
shelf life of EVOO products.

1. Introduction final product [15], which could greatly change the chemical
composition of the oil, leading to unpleasant off-flavors and
Known as a key component in the Mediterranean diet for eventually degrading the quality.
centuries, extra virgin olive oil (EVOO) has become globally For consumers, one of the most important characteristics
recognized and appreciated by consumers due to its unique in EVOO is freshness, as freshness is typically associated with
sensory characteristics and high nutritional values. In recent high quality and ensures food safety [16]. The term “shelf life”
years, there has been considerable interests in correlating is commonly referred to when determining the freshness and
monounsaturated fatty acids (mainly oleic acid) and minor consumer acceptability of EVOO [17]. Specifically, EVOO
components (phenolic compounds, alpha-tocopherol and shelf life could be defined as the length of time under normal
carotenoids, squalene, simple triterpenes, and volatile com- storage conditions within which no off-flavors or defects are
pounds) in EVOO with health benefits {e.g., antihypertensive developed and quality parameters are within accepted limits
activity [1], chemopreventive activity [2], tumor-inhibitory for this commercial category [18]. Consumers rely on shelf-
activity [3], and anti-inflammatory activity [4]} and positive life determinations to differentiate between products that are
sensory attributes [5–7]. However, due to high levels of unsat- acceptable for consumption from those that are no longer
urated fatty acids and the presence of endogenous enzymes acceptable. Thus, it is obligatory for the olive oil industry
such as lipase, polyphenol oxidase, and peroxidase, EVOO to monitor oil quality throughout the production line [19]
is also prone to lipid oxidation and enzymatic hydrolysis and to be able to provide realistic information on shelf-life
which favors autoxidation [8–10]. EVOO oxidation is highly prediction considering the temperature changes and light
dependent on factors including the storage of olive fruit exposure during transport and commercial activities [20].
prior to processing [11], the techniques of oil extraction EVOO shelf-life testing is often conducted under real-
[12], the exposure degree of oxygen, light, and temperature time conditions or accelerated conditions [21]. Real-time
[13], and the packaging [14] and storage conditions of the shelf-life testing allows data collection under normal storage
2 Journal of Food Quality

conditions and reflects actual changes in EVOO matrix over than real-time storage condition monitoring, some acceler-
time [22]. On the other hand, this process requires consistent ated conditions may lead to erroneous shelf-life predictions
storage conditions and can be extremely time consuming because of complicated chemical reaction mechanisms from
when the quality depletion of EVOO proceeds fairly slowly real-time conditions [33]. Thus, shelf-life prediction models
under normal storage conditions [21]. Hence, accelerated are best developed based on results from both real-time
shelf-life testing (ASLT) methods such as Rancimat, Active and accelerated storage conditions, followed by extensive
Oxygen Method (AOM), and Oil Stability Index (OSI) are evaluation and adjustment.
also employed to determine EVOO shelf life under conditions Table 2 provides a summary of olive oil sample size,
which are different from normal storage conditions within chemical/sensory analysis, and statistical approach of the ten
a short period of time [23]. Noticeably, as convenient and shelf-life prediction models discussed in this review.
rapid as the accelerated methods can be, Kaya et al. [24]
reported that extrapolation from the Rancimat values led to 2.1. Pagliarini et al. (2000) [20]. This Tuscan EVOO shelf-life
either underprediction or overprediction of the actual shelf prediction model used induction time, hydroxytyrosol, and
life of sunflower and olive oil due to drastic ASLT conditions. tyrosol to predict the time (in days) to reach an acceptable
Nonetheless, analytical data generated from either or both limit of 2.1 for UV 𝐾232 .
conditions can be applied to the development of EVOO shelf- The research team analyzed a total of 37 samples from five
life prediction models. different lots which are categorized in Table 3. The samples
In general, two types of shelf-life prediction models are were subjected to different bottling, transport, and storage
widely used to simulate EVOO degradation: kinetic models conditions in supermarkets, although the authors found that
and empirical models. Kinetic models are developed based the stability of the oil was not significantly affected. This
on how reaction rates in critical chemical parameters (Table 1) could be due to reasons that (1) the oil was stored properly
are influenced by experimental conditions related to variables in the tanks at processing facility in Italy (OL.MA.) before
such as storage time, temperature, and light [20]. Data getting bottled; (2) the oil did not experience extreme travel
describing the changes of these parameters under conditions stress during transportation to either Italian supermarket
simulating actual storage are submitted to modeling based or Australia supermarket; (3) while the oil was stored in
on the known rate of a particular reaction. The limitation supermarkets, the uncontrolled light and temperature were
of kinetic modeling is that classical kinetic equations cannot still in favor of maintaining the quality of olive oil.
easily accommodate the complexity of oxidation reactions The research team tracked the changes in oil during stor-
and oil deteriorations. Empirical models are developed based age with 21 physiochemical parameters and sensory analysis
on the correlations between individual chemical parameters and via multivariate analysis procedure, it was concluded that
and experimental condition variables. Typically, advanced the most significant parameters were 𝐾232 , induction time,
statistical analyses are performed on analytical data to chlorophyll, carotenoid, alpha-tocopherol, hydroxytyrosol,
develop regression models which enable the prediction of and tyrosol. Since the only parameter that had established
maximum shelf life as a function of chemical parameters limit in the standards was 𝐾232 , three empirical models were
[20, 25]. The limitation of empirical modeling is the difficulty set up to predict the time to reach a given value for 𝐾232 and
to extend beyond the measured setup (e.g., storage condition) 2.1 was chosen as a reference value:
and simplification and approximation can fail when the setup
is changed. (a) 𝑡 = 1130.84Ln (induction time) − 2388.13
Previous studies have been done intensively on how (b) 𝑡 = 329.02 − 38.11 (hydroxytyrosol) (1)
different ratios of chemical composition, packaging systems,
and storage conditions would affect the quality of EVOO (c) 𝑡 = 580.34 − 68.11 (tyrosol) .
[14, 26–31]. However, the olive oil industry is still in great need
of practical and effective shelf-life prediction models that can In these equations 𝑡 is the time (in days) to reach an acceptable
be easily used or adopted after moderate modifications in limit of 2.1 for 𝐾232 . According to the authors, this model
order to reasonably predict EVOO shelf life and to ensure the underestimates the experimental storage time by 20 days for
EVOO products complying with the current regulations for Rancimat induction time, 10 days for hydroxytyrosol content,
its category [32]. and 5 days for tyrosol content.
In this review, ten shelf-life prediction models using var- The above models could be useful for selecting new
ious parameters and approaches are discussed. In addition, olive/oil suppliers and comparing different suppliers, olive
future directions of shelf-life prediction models are proposed harvest years, and storage conditions. While these three equa-
aiming at minimizing the discrepancies between real-time tions consist of simple calculations, the output of estimated
shelf life and predicted shelf life of EVOO products. time is when 𝐾232 reaches 2.1 instead of 2.50 which is the
upper limit of 𝐾232 for EVOO category in the International
2. Prediction Models for EVOO Olive Council (IOC) trade standard [32]. Hence, the results
may not be reflective and reliable in their current form.
Shelf-Life Determination
The development process of EVOO shelf-life prediction 2.2. Gutiérrez and Fernández (2002) [35]. The quality indices
models is streamlined in Figure 1. While ASLT provides a (specified in the European Union standards EC1991 Reg-
more rapid and less-expensive method of predicting shelf life ulation 2568/91) of EVOO samples produced from two
Journal of Food Quality 3

Table 1: Critical chemical parameters used in olive oil shelf-life prediction model development.

Parameter Determination Indicator Methodology

An elevated level of free fatty acid
Free fatty acids are formed by the indicates hydrolyzed fruits
Free fatty acids (FFA) hydrolysis of triglycerides during and/or poor quality oil made Analytical titration
ripening, processing and storage from unsound fruit, improperly
processed or stored oil
Peroxides are primary oxidation
products that are formed when An elevated level of peroxides
Peroxide value (PV) oils are exposed to oxygen, indicates oxidized and/or poor Analytical titration
producing undesirable flavors quality oil
and aroma
Conjugated double bonds are
formed from natural
nonconjugated unsaturation in An elevated level of UV
Ultraviolet
oils upon oxidation. The 𝐾232 absorbance indicates oxidized UV spectrophotometry
absorbance (UV)
measures primary oxidation and/or poor quality oil
products and 𝐾270 measures
secondary oxidation products
Fresh EVOO contains a high
proportion of 1,2-diacylglycerols A low ratio of 1,2-diacylglycerols
to 1,2- and 1,3-diacylglycerols, to 1,2- and 1,3-diacylglycerols is
1, 2-Diacylglycerols
while olive oil from poor quality an indicator for oil that is Gas chromatography (GC)
(DAGs)
fruits and refined olive oils have hydrolyzed, oxidized, and/or of
higher level of 1,3-DAGs than poor quality
fresh EVOO
An elevated ratio of pheophytin a
Chlorophyll pigments break
to pyropheophytins is an
Pyropheophytins down to pheophytins and then High performance liquid
indicator for oil that is oxidized
(PPP) pyropheophytins upon thermal chromatography (HPLC)
and/or adulterated with refined
degradation and aging of olive oil
oil
Sensory evaluation can help
A recognized panel of 8–12
Sensory refers to flavor and identify oils that are of poor
Sensory evaluation people evaluates oils for sensory
aroma attributes quality, oxidized, and/or
characteristics
adulterated with other oils
The oxidation process is Oxidative stability (in hours)
accelerated by means of heating denotes the resistance of oils to
Induction time up the reaction vessel while oxidation. The longer the Rancimat
passing air continuously through induction time, the more stable
the sample the oil
A low level of total phenols can
The sum of up to 30 individual UV spectrophotometry/High
indicate a shorter shelf life while
Total phenols phenols which have antioxidative performance liquid
a high level of total phenols can
ability chromatography (HPLC)
indicate a longer shelf life
Volatile compositions change
during oxidation. For example, as
Volatiles (e.g. The ratios of hexanal/nonanal
the oil oxidizes, the Headspace-gas chromatography
hexanal/nonanal, and E-2-hexenal/hexanal can
concentration of hexanal (GC)
E-2-hexenal/hexanal), indicate oxidized oil
decreases while concentration of
nonanal increases
Saturated and unsaturated fatty
acids consist of the principal
components of fats. Fatty acid Analysis of the fatty acid profile
profiles are distinguishable provides information on the
Fatty acid profile
markers between olive oils and authenticity of the olive oil and Gas chromatography (GC)
(FAP)
some seed/nut oils (FAPs vary can be used as an indicator for
slightly depending on the adulteration
varieties and growing region of
olives)
4 Journal of Food Quality

Select Evaluate Develop Test

Critical Changes in Shelf-life Prediction

chemical products under models based models and
parameters and on the results
real-time and make
their from real-time
accelerated adjustment
acceptable and accelerated
storage based on the
limits related to storage
conditions known data
shelf life conditions

Figure 1: Shelf-life prediction model development process.

cultivars, Picual and Hojiblanca, were monitored throughout 2.3. Psomiadou et al. (2003) [19]. To establish this empiri-
two different storage conditions, together with the evolution cal model, fifty-two Greek virgin olive oil (VOO) samples
of the oxidative stability and sterols, polyphenols, alpha- (Koroneiki cv) from three consecutive crops (1994–1997)
tocopherol, chlorophyllic and carotenoid pigments, and FAP. were obtained as the training set for quality parameters
In this study, a total of 46 L of EVOO was extracted and measurement. The measured parameters included FFA, PV,
packed for each cultivar in Spain. Thirty-four 1 L transparent UV, FAP, and the ratio of unsaturated and saturated fatty
glass bottles of each cultivar were stored inside a thermostated acids, alpha-tocopherol, total phenols, total chlorophylls,
chamber at 30∘ C with illumination (800 lx; 12 h/day), which and OSI. Collinearity diagnostics, variable selection, and
was similar to commercial storage conditions. Other twelve regression analysis were performed on the obtained analytical
bottles of each cultivar were stored at 2∘ C in darkness. In data to determine the contribution of each parameter to
addition, 30 L EVOO of each cultivar was purchased in a maintaining VOO quality.
local market as commercial reference samples and stored Through statistical analyses, the research team located
in the thermostated room. Bottles were sampled weekly alpha-tocopherol, PV, total chlorophylls, and total phenols to
during the first 70 days and subsequently every 15 days for be the most important factors that affected OSI values and
6 months of storage. It is worth mentioning that the EVOO yielded below model:
samples produced from each cultivar had similar initial
values on most of the chemical parameters other than acidity OSI = 5.081 + 0.0102 (alpha-tocopherol)
(Picual: 0.44%; Hojiblanca: 0.26%), stability (Picual: 69.5 h;
− 0.364 (PV) + 0.0477 (total chlorophylls) (2)
Hojiblanca: 43.3 h), and o-diphenols (Picual: 9.00 mg/kg;
Hojiblanca: 14.64 mg/kg). + 0.0259 (total phenols) .
Overall, samples stored at 2∘ C in darkness remained min-
imal to unaltered throughout the entire storage period. Thus, As shown in the above model, all antioxidants contributed in
the regression analysis was performed on selected chemical a similar way to the OSI factor while PV posed clear negative
parameters from samples stored at 30∘ C with illumination for impact on the oxidative stability of the oil. The predictability
each cultivar (Table 3). Similar changes in PV of two olive of this model was further examined and confirmed by a test
cultivars were observed in a 2-fold increase during the first 21 set of 13 VOO samples of the same cultivar from 1999-2000
days and followed by a linear decrease until the end of storage. crop, which showed a negligible prediction bias and a low
The evolutions of alpha-tocopherol, chlorophyllic pigments square root of the mean square error of 2.33, indicating an
(CP), total polyphenols (TP), and o-diphenols were well fitted effective prediction of OSI was achieved in this model for
to first-order kinetics. Most importantly, the coefficient 𝐾270 , VOO of Koroneiki cv.
which measures the accumulation of secondary oxidation In this study, the effect of many oxidative parameters
products that cause off-flavors in olive oil, showed a sharp on oils from different crop years was examined with com-
increase along the storage period in all the samples stored at prehensive statistical analyses, yielding a simple predictive
30∘ C with illumination in spite of cultivar and sample source. equation, and followed by validation on another 13 samples
As a result, an excellent correlation between initial stability from the same cultivar. However, while this model gives
and time to reach the limit of 𝐾270 = 0.25 was established for useful information regarding the oil stability which impacts
EVOO samples bottled in glass containers regardless of olive shelf life directly, it would require producers to incur the
cultivar (Table 4). expense for three tests (alpha-tocopherol, total phenols, and
The correlation between initial stability (𝑆) and storage total chlorophylls) that are not currently required in the
time to achieve 𝐾270 of 0.25 has demonstrated when an standards [32]. Besides, producers can request OSI analysis
EVOO no longer retains its extra virgin quality. Being a (by Rancimat) for less of the cost than these three tests
critical indicator of oxidation level, 𝐾270 is required by the although the correlation between OSI and actual shelf life
IOC standard [32] and can be easily obtained by producers. was not elaborated. Regardless, this model still has practical
Nonetheless, the validation of this model is in need for other influence on the routine control of Koroneiki cv VOO in the
cultivars with a larger sample size in an extended storage industry and future development of prediction models for
period. Storage containers other than glass type should also VOO made from other olive cultivars can be derived from
be taken into consideration when applying this model. this validated model with minor modifications.
 Journal of Food Quality

Table 2: Summary of shelf-life prediction models discussed in the review.

Model Sample (bottles) Storage condition Chemical/physical analysis Sensory analysis Statistical analysis Shelf-life prediction indicator Ref.
FFA, PV, UV, polyphenol, (i) Sample classification: principal component
(i) Dark glass
alpha-tocopherol, tyrosol and analysis (PCA) and partial least-squares
(ii) In the dark Time (in days) to reach 𝐾232 of 2.1 (𝑡):
hydroxytyrosol, secoiridoid analysis (PLS) on Unscrambler 6.0 software
(20∘ C)/uncontrolled light and (i) 12 trained panelists (i) 𝑡 = 1130.84 Ln (induction time) − 2388.13 Pagliarini et al.
1 37 Tuscan EVOO from 5 Lots aglycons, chlorophyll package (Camo As, Trondheim, Norway)
temperature (ii) Bitterness and astringency (ii) 𝑡 = 329.02 − 38.11 (hydroxytyrosol) (2000) [20]
absorbance, carotenoid (ii) Comparison of regression lines:
(iii) 14/16/17/21 months; sampled (iii) 𝑡 = 580.34 − 68.11 (tyrosol)
absorbance, induction time Statgraphics Plus 1.0 software package
every 2 months
(120∘ C, 20 L/h) (Manugest KS Inc., Rockville, MD)
(i) Clear glass
46 experimental Spanish FFA, PV, UV, total phenols,
(ii) Thermostated chamber (i) Comparison of means: Duncan’s test
Picual and Hojiblanca o-diphenols, tocopherols, (i) 12 trained panelists Time (in days) to reach 𝐾270 of 0.25(𝑡) according to initial Gutiérrez and
(30∘ C)/in the dark (2∘ C) (ii) Analysis of variance and correlation:
2 EVOO and 30 commercial chlorophyllic and carotenoids, (ii) Highest quality (score 9) to stability (𝑆): Fernández (2002)
(iii) 6 months; sampled weekly CoStat 2.10 software (CoHort Software,
Picual and Hojiblanca FAP and sterols, induction time lowest quality (score 1) 𝑆 = 1.01𝑡 − 12.84 [35]
during the first 70 days and every Berkeley, CA)
EVOO (100∘ C, 10 L/h)
15 days afterward
(i) Effect of the production year: linear
regression, 𝑡-test and variable selection
(ii) Possible collinearity among independent
variables: variance inflation factor (VIF), PCA
52 Greek Koroneiki virgin FFA, PV, UV, total phenols, and singular value decomposition (SVD)
olive oil (VOO) from 1994 to alpha-tocopherol, total (iii) Selection of analytical parameter
1997 for model development chlorophylls, FAP and the ratio affecting OSI the most: regressions, forward OSI = 5.081 + 0.0102 (alpha-tocopherol) − 0.364 (PV) + Psomiadou et al.
3 Stored at −22∘ C till analysis NP∗
and 13 Koroneiki VOO from of unsaturated and saturated fatty and backward selection, stepwise selection, 0.0477 (total chlorophylls) + 0.0259 (total phenols) (2003) [19]
1999-2000 for model acids (U/S), induction time Mallow’s index and Akaike’s information
validation (120∘ C, 20 L/h) criterion (AIC)
(iv) Statistical packages: SAS version 8 (SAS
Institute Inc., Cary, NC), SPSS version 10
(IBM Corporation, Chicago, IL), and JMP IN
version 3.1.7 (SAS Institute Inc., Cary, NC)
Large EVOO sample size
63 chemical parameters (i) 25 trained panelists
from Mediterranean areas (i) Fractional factorial design (FFD): Modde EVOO degradation parameter value (𝑌) as a function of
including FFA, PV, UV, minor (ii) 18 sensory parameters
from 1999 to 2001 for model 8.0 software package (Umetri, Umea, Sweden) FFA (𝑋1 ), oleic acid content (𝑋2 ) and bitterness score Zanoni et al. (2005)
4 NP component content, lipid including green olive
development and 11 EVOO (ii) PCA and PLS: Unscrambler 7.8 software (𝑋3 ): [10]
oxidation status and antioxidant aroma/flavor (e.g. bitterness),
from 2002 for model package (Camo AS, Oslo, Norway) 𝑌 = 𝑐+𝑎1 𝑋1 +𝑎2 𝑋2 +𝑎3 𝑋3 +𝑎4 𝑋1 𝑋2 +𝑎5 𝑋1 𝑋3 +𝑎6 𝑋2 𝑋3
activity astringency, and pungency
validation
(i) Determination of differences between
treatments for the hexanal evolution rate: SAS
(i) PET/PVC/glass bottle Probability for the olive oil to reach the end of its shelf life
8.2
(ii) Covered with aluminum foil
(ii) Separation of the means of GC areas: during a certain period of time (𝑃safe ): Coutelieris and
432 Portuguese organic inside fiberboard boxes/under 𝑡
5 Hexanal NP Tukey test and Duncan test Kanavouras (2006)
EVOO fluorescent light at 15/30/40∘ C ∫𝑡 2 ⟨𝐶hexanal ⟩ (𝑡) 𝑑𝑡
1
(iii) Model development: nonuniform 𝑃safe = 1 − [34, 36]
with relative humidity of 60% 𝑡
finite-difference scheme with an upwinding ∫0 2 ⟨𝐶hexanal ⟩ (𝑡) 𝑑𝑡
(iii) 12 months; sampled monthly
numerical algorithm (Newton method for
nonlinear systems)
5
 6

Table 2: Continued.
Model Sample (bottles) Storage condition Chemical/physical analysis Sensory analysis Statistical analysis Shelf-life prediction indicator Ref.
(i) Differences between treatments: Duncan
test on SPSS version 14
(ii) Linear and nonlinear regression:
(i) Opened amber glass GraphPad Prism 4.02 (GraphPad Software,
PV, UV, FAP, phenolic Time (in weeks) to reach 𝐾232 of 2.5 at a mild temperature
Seven Spanish Cornicabra (ii) In the dark at 25/40/50/60∘ C Inc., San Diego, CA) (T ≤ 60∘ C): Mancebo-Campos et
6 compounds, tocopherols, NP
VOO (iii) sampled after 93/41/34/19 (iii) Oxidation and antioxidant degradation al. (2008) [23]
induction time (100∘ C, 10 L/h) TRUL = 𝑎𝑇𝑏
weeks rates: calculated from the slopes of respective
concentration versus time curve
(iv) Effect of temperature on rates of
oxidation: Arrhenius equation
The percentage of pyropheophytin a (% PPP) over time
(𝑡): % PPP (𝑡) =
(i) Differences between means: one-way ((𝑒(𝑎1 −𝛽1 /𝑇) [PP]0 / (𝑒(𝛼2 −𝛽2 /𝑇) − 𝑒(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) ))
ANOVA
(i) Amber glass (𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )𝑡 (𝛼2 −𝛽2 /𝑇) )𝑡
Chlorophyll pigments (ii) Post hoc comparison: Brown and Forsythe ⋅ [𝑒−(𝑒 − 𝑒−(𝑒 ])
(ii) In the dark at room Aparicio-Ruiz et al.
7 Six single-cultivar VOO (pheophytin a and NP test [37]
temperature/15∘ C (𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )𝑡 (2012) [16]
pyropheophytin a) (iii) PCA, PLS, and nonlinear regression: × ([PP]0 𝑒−(𝑒
(iii) 12 months; sampled monthly
Statistica 6.0 and Statgraphics Centurion XV
for Windows (StatSoft Inc., Round Rock, TX) + (𝑒(𝑎1 −𝛽1 /𝑇) [PP]0 / (𝑒(𝛼2 −𝛽2 /𝑇) − 𝑒(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) ))
(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )𝑡 (𝛼2 −𝛽2 /𝑇) )𝑡 −1
⋅ [𝑒−(𝑒 − 𝑒−(𝑒 ])
FFA, PV, total tocopherols and Calculate shelf life at 50∘ C (SL50 ) as a function of
total phenols, total polar induction time (OSI):
ANOVA and regression analyses: MStatC
compounds, conjugated diene 100 − 𝑎0 Farhoosh and
(Michigan State University, East Lansing, MI) SL50 = 0.9985 {𝐴 ( ) (OSI − 𝑏)
8 Nine olive oil samples Stored at 4∘ C until analysis value, ratio of mono- and NP 100𝑎 Hoseini-Yazdi (2013)
and SlideWrite (Sigma Aldrich, St. Louis,
poly-unsaturated fatty acids [25]
MO) 𝑎1 ((𝑏 − OSI) /100𝑎)
(M/P ratio), and induction time +𝐴 + 𝐵}
(100/110/120/130∘ C, 25 L/h) 2
1 + ((OSI − 𝑏 − 𝑎𝑎2 ) /𝑎𝑎3 )
Best before date (in months) from the lowest value
obtained from induction time, DAGs, FFA Factor (derived
(i) Dark glass from FFA) and PPP:
A wide range of commercial
(i) 12 trained panelists (a) Hours of induction time at 110∘ C
olive oil samples for model (ii) In the dark at 18 ± 2∘ C DAGs − 35%
FFA, PV, UV, PPP, DAGs, and (ii) The median values of defect, Guillaume and
9 development and 118 olive oil (iii) 30 months; sampled when NP (b)
induction time (110∘ C, 20 L/h) fruitiness, bitterness, and FFA Factor Ravetti (2016) [18]
and 20 EVOO for model estimated best before date was FFA factor = 1.7% (if FFA < 0.4%); 2.1% (if FFA > 0.4%
pungency
evaluation reached and <0.6%); or 2.5% (if FFA > 0.6%)
17% − PPPs
(c)
0.6%
(i) Amber glass
(ii) In the dark/exposed to (i) 4 trained panelists
natural and artificial light at (ii) Olfactory sensations,
FFA, PV, UV, induction time; 3 best linear discriminant analysis (LDA) and simulated Rodrigues et al.
10 36 EVOO gustatory-retronasal sensations, See Table 10
room temperature (17–25∘ C) electronic tongue signal profile annealing (SA) prediction models (2017) [38]
and final olfactory-gustatory
(iii) 12 months; sampled after sensations
0/3/6/9/12 months
∗
NP: not provided.
Journal of Food Quality
Journal of Food Quality 7

Table 3: Sample Lot information in the Pagliarini et al. (2000) model.

Lot 𝐴
Lot # Lot 𝐵1 Lot 𝐵2 Lot 𝐶1 Lot 𝐶2
(reference lot)
Time taken from Immediately after After 77 days of After 188 days of After 98 days of After 188 days of
freshly made batch processing storage in tanks storage in tanks storage in tanks storage in tanks
100 mL dark glass, 500 mL dark glass, 500 mL dark glass, 500 mL dark glass, 500 mL dark glass,
Bottling closed with screw closed with screw closed with screw closed with screw closed with screw
caps caps caps caps caps
Shipping A supermarket in A supermarket in
Processing facility A supermarket in A supermarket in
destination after Italy (close to Italy (close to
in Italy (OL.MA.) Australia Australia
bottling OL.MA.) OL.MA.)
Storage condition Uncontrolled light Uncontrolled light Uncontrolled light Uncontrolled light
In the dark at 20∘ C
at destination and temperature and temperature and temperature and temperature
Storage period at
21 months 16 months 14 months 17 months 14 months
destination

Table 4: Correlations between storage time 𝑡 (in days) and selected Combining the results from PCA mapping and PLS
parameters by Gutiérrez and Fernández (2002). modeling has proved the hypothesis that in EVOO samples
(1) the more acidity the more degradation; (2) the more
Cultivar Picual Hojiblanca oleic acid content the less degradation; and (3) the more
PV = bitter the taste the less the degradation. Furthermore, PV, UV
PV = −0.04𝑡 + 7.2;
PV (mequiv/kg) −0.03𝑡 + 6.6; 𝐾232 , and lipid oxidation status (oxidized fatty acid content
𝑟 = 0.9532
𝑟 = 0.9600
at 230 nm and dienoic and trienoic conjugated fatty acids
Ln (% TP) = Ln (% TP) = content) were found to be the most critical parameters when
TP (mg/kg, caffeic acid) −4.45×10−3 𝑡+2.03; −2.55 × 10−3 𝑡 + measuring EVOO degradation. A mathematical model was
𝑟 = 0.9879 1.97; 𝑟 = 0.9965
established to predict EVOO degradation as a function of the
Ln (CP) = Ln (CP) = combination of the three most relevant indices (acidity, oleic
CP (mg/kg) −0.11𝑡 + 12.34; −0.26t + 18.92;
acid content, and bitter taste):
𝑟 = 0.9848 𝑟 = 0.9810
Initial stability (𝑆) for the 𝑌 = 𝑐 + 𝑎1 𝑋1 + 𝑎2 𝑋2 + 𝑎3 𝑋3 + 𝑎4 𝑋1 𝑋2 + 𝑎5 𝑋1 𝑋3
achievement of 𝐾270 = 0.25 𝑆 = 1.01𝑡 − 12.84; 𝑟 = 0.9823 (3)
(h) + 𝑎6 𝑋2 𝑋3 ,

where 𝑌 is the selected degradation parameter to be pre-

2.4. Zanoni et al. (2005) [10]. A phenomenological model dicted, 𝑋1 is the acidity, 𝑋2 is the oleic acid content, and 𝑋3
was introduced for the first time to predict the stability of is bitter taste score. Constant values a𝑥 are listed in Table 5.
EVOO based on combined stability/instability composition Unlike what had been found in previous studies [19, 20,
indices. The experimental design comprised two steps: (1) 35], the antioxidant component content which consisted of
stability/instability indices screening and (2) significant rela- antioxidant activity and minor polar component content in
tionships between screened indices and EVOO degradation this study showed insignificant impact on EVOO degradation
investigation and confirmation. The screening of composi- and was excluded from the proposed model as a result.
tion indices was carried out by multivariate analysis on data Predictive models of oil degradation degree can be
derived from 63 chemical and 18 sensory parameters obtained obtained based off of the above proposed mathematical
from oils purchased from four different Mediterranean area model, which may be useful to predict the rate of oil
during the 1999–2001 crops. Based on the statistical analysis, degradation if the oil degradation history was known. In this
the research group proposed that acidity value was indirectly regard, a major limitation of this model is that it was based
related to oil stability while oleic acid content and bitter on constant indices without taking the composition changes
taste were directly related to oil stability. The predictability under storage conditions into full consideration. That is,
of these most relevant indices to oil stability was then any changes of oil composition that occurred during lipid
checked by measuring six major degradation parameters oxidation would require a new set of quality index values to
on eleven oil samples differing in screened indices planned maintain the model validation. Although this drawback may
by a fractional factorial design (FFD) and processed with be overcome by replicating the experimental design several
principal component analysis (PCA) and partial least squares times, the application of this model may be limited to EVOO
(PLS) regression afterward. Parameters of PV, UV, minor samples being stored under optimal conditions that have
polar component content (oleuropein and ligstroside deriva- minimal effects on the change of stability/instability indices
tives), oxidative status of fatty acids, antioxidant activity, and and/or samples that yield similar rate of degradation kinetics
sensory evaluation were measured in this step. for the same stability/instability indices combination.
8 Journal of Food Quality

Table 5: Constant values of selected degradation parameters for empirical polynomial models by Zanoni et al. (2005) [10].

Degradation parameter 𝑐 𝑎1 𝑎2 𝑎3 𝑎4 𝑎5 𝑎6
PV −77.921 115.143 1.148 28.910 −1.411 −3.679 −0.367
𝐾232 −6.364 10.911 0.106 2.981 −0.133 −0.328 −0.037
Lipid oxidation status
Dienoic trans-trans −0.051 −0.103 0.002 0.136 0.002 −0.040 −0.001
Dienoic cis-trans, trans-cis 0.990 −0.510 0.006 0.054 0.023 −0.262 −0.002
Trienoic conjugated fatty acid content −1.562 2.960 0.020 0.563 −0.034 −0.183 −0.006
Oxidized fatty acid content at 230 nm −0.280 4.805 0.032 1.164 −0.054 −0.099 −0.020

Table 6: Sample packaging and storage conditions for a 12-month study in the Coutelieris and Kanavouras (2006) model.

Sample Portuguese organic EVOO

Packaging material 0.5 L PET bottle 0.5 L PVC bottle 0.5 L glass bottle
Oxygen transmission rate at 0.21 atm driving force (cc/m2 /day) 8 9.8 N/A
Half covered with aluminum foil inside fiberboard boxes; half
Storage location
exposed to fluorescent light
Storage temperature (∘ C) 15, 30, and 40
Relative humidity (%) 60

2.5. Coutelieris and Kanavouras (2006) [34, 36]. As listed in

Table 1, volatile compounds are good indicators of olive oil
quality as they are mainly produced through lipoxygenase
pathway and chemical oxidation during processing and
⟨＃Ｂ？Ｒ；Ｈ；Ｆ ⟩ oil

B
storage and contribute greatly to the olive oil flavor [39]. In
this study, the evolution of hydroperoxide in the packaged t1 t2
Portuguese organic EVOO samples was monitored and the
progression of hexanal, which was assumed as the most A
prominent volatile compound posing higher impact on the
sensory attributes of olive oil, was quantified over a 12-month
storage period. Table 6 shows the packaging materials and 0 2 4 6 8 10 12
storage conditions of analyzed EVOO samples. Time (months)
A mathematical model for the mass transfer taking place
in the oil-package material interacting system was deduced Figure 2: The graphical representation of the definition of 𝑃safe .
based on four assumptions in the oil phase and two assump- The threshold of the hexanal concentration is represented by the
long dash dot line {adopted from Coutelieris and Kanavouras (2006)
tions in the oil-package system. In the oil phase, the assump- [34]}.
tions were (1) the oil quiescent; (2) all the hydroperoxides
eventually transformed to hexanal during lipid oxidation; (3)
at time (𝑡) = 0, there was a measurable amount of oxygen, The study showed that samples kept under light had
fatty acid, and hexanal in the oil phase; and (4) the packaging yielded much higher concentration of hexanal when com-
materials adsorbed hexanal according to Langmuir isotherm. pared to the samples stored in dark. In addition, the highest
In the oil-package system, the assumptions included the hexanal concentration was found in samples stored in PET
following: (1) oxygen and hexanal had constant concentration bottles at 40∘ C with light exposure, followed by those stored
outside the bottles at spatial coordinate (𝑥) = 0; and (2) in glass, and samples stored in PVC bottles had a lower
hexanal concentration. As shown in Figure 2, 𝑃safe , the
at 𝑡 = 0, oxygen and hexanal concentrations inside the
probability for the olive oil to reach the end of its shelf life
packaging material were zero. The mass transfer phenomena
during a certain time period is comparable to the ratio of the
were elaborated explicitly by using diffusion equations for dif-
areas below (area A) and above (area B) a roughly defined
fusion of oxygen and hexanal and Langmuir-type adsorption threshold of the hexanal concentration (long dash dot line).
for hexanal adsorption in the oil-package (cylinder bottle) The estimation of 𝑃safe was proposed in the following model
system. A numerical algorithm, along with a nonuniform during the same time period [𝑡1 , 𝑡2 ]:
finite-difference scheme, was then applied with modifications
to solve the issue of nonlinearity of the studied system for 𝑡
∫𝑡 2 ⟨𝐶hexanal ⟩ (𝑡) 𝑑𝑡
various combinations of the storage conditions mentioned in 𝑃safe = 1 − 1
𝑡2 , (4)
Table 6. ∫0 ⟨𝐶hexanal ⟩ (𝑡) 𝑑𝑡
Journal of Food Quality 9

where 𝐶hexanal is the concentration of hexanal, 𝑡1 is the time 5.0

when concentration reaches the upper limit for the oil’s
quality acceptance, 𝑡2 is set to 12 months in this study, and the 4.0
brackets indicate spatial averaging of hexanal concentration
being used. 3.0

Ln TRUL
The sensitivity of this model was tested on samples kept
under different storage conditions and 𝑃safe values were 2.0
compared for four different thresholds (15%, 20%, 25%,
and 30% over the initial hexanal concentration). One of 1.0
the key findings suggested that the predictions diverged
from experimental results under specific storage conditions
0.0
due to the low concentrations of hexanal in oil stored in 3.0 3.2 3.4 3.6 3.8 4.0 4.2
dark at any temperature. Moreover, the determination of Ln Temperature
hexanal concentration threshold was ambiguous without
knowing data generated from additional chemical analyses Figure 3: Correlation between TRUL and temperature for 𝐾232
and sensory evaluation. Most importantly, the amount of (TRUL = 𝑎𝑇𝑏 ). Seven samples denoted in seven shades {adopted
hexanal does not always allow oxidized olive oils to be distin- from Mancebo-Campos et al. (2008) [23]}.
guished from virgin ones, as this compound can come from
both lipoxygenase and oxidative pathways [40]. Nonetheless,
the proposed model had undertaken a comprehensive and
extensive investigation on the EVOO degradation in the oil- first-order kinetics. Furthermore, the polyunsaturated fatty
package system by factoring in the chemical reactions and acids (PUFA) linoleic and linolenic acids showed a linear
diffusion of compounds both in the oil phase and through decrease at a rate increasing with storage temperature, and
packaging materials, granting a promising parameter for the best correlation was drawn between loss of PUFA and
better monitoring the shelf life of packaged olive oil stored increase of 𝐾232 at all temperatures as described by the linear
under various conditions. The validation of 𝑃safe model can Arrhenius equation.
be further strengthened by adding sensory analysis. As a good indicator of primary oxidation level and an
easy parameter to determine, 𝐾232 showed high linearity
in the early stages of oxidation and presented excellent
2.6. Mancebo-Campos et al. (2008) [23]. During the storage
of seven Cornicabra cv VOO samples (varied in total phenol correlation with loss of UFA. Thus, 𝐾232 was selected as
concentrations) in dark and at mild temperatures (25, 40, the best normalized oxidation index for potential shelf-life
50, and 60∘ C), the autoxidation kinetic behavior of the main estimation of VOO, defined as TRUL, at a mild temperature
oxidation indices (PV, 𝐾232 , and 𝐾270 ) and the oxidizing (≤60∘ C):
substrate [unsaturated fatty acids (UFA)] were reported for
the first time. In addition, the extrapolated time (in weeks) TRUL = 𝑎𝑇𝑏 . (5)
required to reach the upper limit (TRUL) of each main
oxidation index in the EU regulation for the VOO category
was also calculated based on the experimental results from Based on the TRUL results of 𝐾232 generated at different
this study and a previous study conducted by the same temperatures, the above model can be further explained by
research group [41]. Figure 3. As a result, the predicted TRUL at 25∘ C was very
According to the evolution of measurements in this study, close to the experimental TRUL at the same temperature
PV did not reach its upper limit (20 meq/kg) in any samples when applying the proposed model to accelerated storage
stored at 25∘ C by the end of a 93-week storage, nor did it do temperatures (40, 50 and 60∘ C).
that in some of the samples stored at higher temperatures. Unlike drastic ASLT conditions where olive oil samples
Stabilization of PV was reached below or slightly above the are tested on oxidative stability at over 100∘ C [43, 44],
limit in all cases in spite of more harsh storage temperatures this model conducts an accelerated stability test at mild
and intensive air exposure in opened bottles. This similar temperatures below 60∘ C and allows a time-saving shelf-life
observation was also confirmed by other research groups as prediction to reasonably estimate the actual shelf life of VOO
a reduction in PV would occur due to the breakdown of samples stored under normal storage conditions (25∘ C). It is
peroxides into secondary products [15, 42], indicating the worth noting that VOO samples were stored in open bottles
unreliability of PV being used as a quality marker for olive oil throughout the study with intensive oxygen exposure, which
shelf life. On the contrary, the upper limit of 𝐾232 (2.5 K1% 1 cm ) did not reflect the actual storage conditions from a commer-
was reached in samples stored at any conditions although cial standpoint. Besides, VOO samples used in this study were
𝐾232 and PV tended to stabilize at a similar value in each from the same cultivar with similar initial concentrations on
sample stored at higher temperatures, following pseudo zero- the majority of the measured parameters. A follow-up study
order kinetics before reaching the plateau. On the other hand, focusing on the contribution of antioxidants content and fatty
the upper limit of 𝐾270 (0.22 K1% 1 cm ) was reached in all acids unsaturation degrees to oxidation rates is also necessary
samples with only two exceptions at 25∘ C, yielding pseudo to test the applicability of the proposed model.
10 Journal of Food Quality

2.7. Aparicio-Ruiz et al. (2012) [16]. Chlorophyll pigments 3% (v/v) headspace, in the dark at room temperature. The
are sensitive to small amounts of degradation, which would monthly temperatures range from 10.4∘ C to 28.6∘ C through-
eventually take place in an EVOO even under optimal storage out the year, with an average annual temperature of 19.3 ±
conditions. During storage, pheophytin a (PP) degrades to 1.9∘ C. Chlorophyll pigments were quantified every month up
PPP (Table 1). The ratio of these two compounds therefore is to one year. The degradation of PP was found fitting first-
a useful parameter to track olive oil degradation over time. order kinetics after applying multivariate statistical analysis
This kinetic prediction model is established based on PPP to the experimental data. The statistical results also showed
that time, temperature, and initial PP concentration were
because PPP changes predictably with time under specific
the main variables that affected PPP prediction for shelf life.
temperatures [45].
Percent PPP (% PPP) over time was defined as the quotient of
In developing this model, the research team stored six the concentration of PPP ([PPP]) and the sum of [PPP] and
single-cultivar VOO samples (Blanqueta cv, Arbequina cv, [PP]. A mathematical model to predict % PPP as a function
Cornicabra cv, and Picual cv) in 65 mL amber glass jars with of time and temperature was then developed as shown below:

(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) (𝛼2 −𝛽2 /𝑇)

(𝑒(𝑎1 −𝛽1 /𝑇) [PP]0 / (𝑒(𝛼2 −𝛽2 /𝑇) − 𝑒(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )) [𝑒−(𝑒 )𝑡
− 𝑒−(𝑒 )𝑡
]
% PPP (𝑡) = . (6)
[PP]0 𝑒 −(𝑒(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )𝑡 + (𝑒(𝑎1 −𝛽1 /𝑇) [PP]0 / (𝑒(𝛼2 −𝛽2 /𝑇) − 𝑒(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )) [𝑒 −(𝑒(𝛼𝑡𝑎 −𝛽𝑡𝑎 /𝑇) )𝑡 − 𝑒−(𝑒
(𝛼2 −𝛽2 /𝑇) )𝑡
]

In this equation, [PP]0 is the initial concentration of PP, 𝑇 the storage conditions of VOO. Table 7 shows shelf life (in
is temperature in Kelvin, 𝑡 is the storage time in hour, and months) for VOO samples stored at 10∘ C and 16∘ C before
values 𝛼1 , 𝛽1 , 𝛼2 , and 𝛽2 are related to kinetic constants and reaching the Australian/California upper limit for PPP of
are protected by industrial license according to the authors. 17%. For instance, if % PPP is 0.64% at bottling, the oil will
According to the proposed model, % PPP at any time point have more than 36 months and 21 months before it reaches
can be calculated if the initial PP and PPP concentration and the limit of 17% if stored at 10∘ C and 16∘ C, respectively. These
storage temperature are known. temperatures are likely to be cooler than the actual storage
This study also compared the change of % PPP under temperature; thus a follow-up study with oil stored at a typical
a well-controlled storage temperature of 15∘ C and room store shelf temperature is recommended.
temperature for six single-cultivar VOO samples. Overall, This model only consists of two chlorophyll pigments (PP
and PPP) and can be used to monitor the changes of storage
% PPP increased under both temperatures, indicating the
temperature and to detect undesired storage conditions based
degradation of olive oil quality occurred over time in spite of
on the rate of pyropheophytinization. Knowing the value of
cultivars. However, it is clear that the same samples stored at
% PPP at any moment during a storage period would also
room temperature had a significant increase in % PPP from
allow a timely adjustment on proper storage temperature
0 to above 8%, especially during summer time (6–8 storage
and later on provide a better shelf-life estimation. However,
months) when room temperature was typically higher. The
without knowing the values of other quality parameters
development of this parameter tended to be linear with a
of VOO samples, the % PPP alone may not reflect the
smaller slope (from 0 to 2%) throughout the entire storage
storage condition correctly as light exposure can cause the
period at 15∘ C. This finding confirms the temperature impact
complete breakdown of chlorophylls and all of its derivatives
on PPP generation over time which should be taken into
therefore yield a zero value of % PPP [59]. Hence, inclusion of
consideration when developing the kinetic model.
other quality parameters of samples would benefit the model
After being validated on and compared with another
set of empirical data calculated from chlorophyll pigment optimization.
experimental data obtained by Gallardo-Guerrero, et al. [46],
the model was adopted to develop a % PPP prediction graph 2.8. Farhoosh and Hoseini-Yazdi (2013) [25]. The empirical
between 15∘ C and 35∘ C as shown in Figure 4. The authors model was developed based on the relationship between
suggested that the % PPP acceptable limit could be set at 14%, oxidative stability measurements (OSI) taken at high tem-
which would allow VOO to have one year of shelf life if stored peratures (100–130∘ C) and the chemical composition data
under 22∘ C. However, this value seems arbitrary as it did take obtained at a low temperature (50∘ C).
into account any other chemical parameters and/or sensory To study the contribution of each compositional parame-
results. ter to the oxidative stability in olive oil, nine olive oil samples
In a follow-up study published in 2014 [47], the same in 1 L glass bottles were purchased from local shops and stored
research team applied this % PPP prediction model to single- at 4∘ C until analysis on accelerated stability at 100–130∘ C.
cultivar olive oils (Arbequina cv) with various levels of initial And the ratios between mono- and polyunsaturated fatty
% PPP at bottling. The samples were stored at different acids (M/P ratio), PV and FFA, total tocopherols (TT) and
average annual temperatures, ranging from 10∘ C to 16∘ C. total phenols (TP), total polar compounds (TPC), conjugated
The authors concluded that the initial value of % PPP is of diene value (CDV), and induction period (IP) were tested for
great importance to be included for a better monitoring of the storage stability on the same samples incubated at 50∘ C.
Journal of Food Quality 11

Table 7: Shelf life (in months) for VOO stored at 10∘ C and 16∘ C conditions could lead to over- or underprediction of the
before reaching Australian/California limit of 17% summarized actual shelf life due to complicated kinetics involved at higher
from Aparicio-Ruiz et al. (2014). temperature [24, 33].
Regression models developed under low- (model (a))
Shelf life if stored at Shelf life if stored at
% PPP at bottling and high-temperature (model (b)) were also provided based
10∘ C 16∘ C
on the analytical data generated from either condition. By
0.64 >36 21 incorporating the chemical composition data collected at
1.35 >36 20 50∘ C into the OSI measurement at 100–130∘ C, an empirical
3.26 >36 19 model (c) of shelf-life prediction (SL50 ) was derived from
7.06 34 16 model (a) and model (b):
8.66 30 10
3
(a) SL50 = 24.0639 (∑𝐶𝑖 ∗ 𝑆𝑖 ) + 104.7369, (7)
84
𝑖=1
35∘ C
70
where 𝐶𝑖 and 𝑆𝑖 are regression coefficients and standardized
56 compositional variables.
% PPP

42 30∘ C

28
(b) SL50 = 10(50𝑠+𝑖−1.2272) , (8)
∘
25 C
20∘ C
14
15∘ C
where 𝑠 and 𝑖 values are slopes and intercept of the linear
0 equation to the log OSI versus accelerated temperature.
0 2 4 6 8 10 12
(Month) 100 − 𝑎0
(c) SL50 = 0.9985 {𝐴 ( ) (OSI − 𝑏)
Figure 4: Predicted % PPP during one year of storage at temper- 100𝑎
atures between 15∘ C and 35∘ C {adopted from Aparicio-Ruiz et al. (9)
(2012) [16]}. 𝑎1 ((𝑏 − OSI) /100𝑎)
+𝐴 2
+ 𝐵} ,
1 + ((OSI − 𝑏 − 𝑎𝑎2 ) /𝑎𝑎3 )
During the storage stability test conducted at 50∘ C, the
evolution of hydroperoxides and conjugated dienes showed where 𝑎, 𝑏, 𝐴, and 𝐵 are the values of the linear regression
two pseudo zero-order kinetic curves: a gradual slope of models developed at high and low temperatures, respectively.
linear stage which was considered as the initiation phase The values of 𝑎0 , 𝑎1 , 𝑎2 , and 𝑎3 were calculated and shown
of lipid oxidation and then a steep slope of another linear in Table 8. According to the conclusion of 𝑄10 factor from
stage known as the propagation phase. The storage time (in Mancebo-Campos et al. [23], which is that a decrease of 10∘ C
days) at intersection points of the PV and CDV curves was in the storage temperature increases the shelf life of olive
identified as the induction period IPPV and IPCDV for the olive oil more than two folds, a value of 2.1 of 𝑄10 was used to
oil sample. The level of hydroperoxides increased gradually estimate the oil shelf life at 25∘ C (normal storage temperature)
during IP and then elevated rapidly in the propagation by using the regression model (a) and promising estimation
phase, where decomposition of hydroperoxides to aldehydes, was obtained (13.1–22.2 months) which was considered to
ketones, and other secondary oxidative products occurred be representative of the typical shelf life claimed by olive oil
and off-flavors were accumulated [15]. Thus, the IP-based producers (12–18 months after production).
oxidative stability values IPPV and IPCDV were selected as Model (c) permitted the estimation of olive oil shelf life to
better parameters to measure the oxidative stability and be achieved within acceptable errors less than ±10% by using
determine the shelf life of olive oil at 50∘ C. only one measurement, OSI, at accelerated temperatures. The
Positive correlations were found between oxidative sta- interrelated mathematical equation of the low- and high-
bility (IPCDV at 50∘ C and OSI at 100–130∘ C) and M/P ratio, temperature regression models also allows real-time shelf-
tocopherols, and phenolics. To further elucidate, the higher life prediction from the accelerated testing results to be
the M/P ratio is, the less prone to rancidity the olive oil is; the done rapidly. A limitation of this model is that only two
higher the content of tocopherols and/or phenolics of the oil EVOO samples were analyzed; without performing further
is, the better the antioxidative ability the oil has. It is worth validation on the empirical model on a larger size of EVOO
mentioning that the order of the IP-based oxidative stability samples, the calculated values provided in Table 8 and the
of olive oil samples at 50∘ C was sample 7 > 2 > 6 ≈ 3 > correction coefficient of 0.9985 may considerably deviate and
9 > 4 ≈ 1 > 8 > 5, whereas the order of that determined not reflect the actual situation of EVOO category.
by the OSI from the accelerated stability test at 100–130∘ C
followed sample 7 > 9 > 3 > 8 > 6 ≈ 2 ≈ 1 > 5 > 4. The 2.9. Guillaume and Ravetti (2016) [18]. This empirical model
difference may be indicative of the fact that the extrapolation uses four quality parameters, induction time, DAGs, FFA
from the OSI obtained at accelerated temperature to ambient Factor (derived from FFA), and PPP, to identify a best before
12 Journal of Food Quality

Table 8: The values of 𝑎0 , 𝑎1 , 𝑎2 , and 𝑎3 in the SL50 prediction model calculated at 100∘ C and 130∘ C by Farhoosh and Hoseini-Yazdi (2013).

Temperature (∘ C) 𝑎0 𝑎1 𝑎2 𝑎3
100 −174.4761 −201.4675 32898.6507 19757.9412
130 0.0108 0.0230 −0.0106 0.0190

date (BBD, in months) using the lowest value obtained from Table 9: Recommended packaging and storage conditions for olive
the following three equations: oil shelf life.

(a) Hours of induction time at 110∘ C Packaging Temperature Light

Dark glass, aluminum cans with
DAGs − 35% (10)
food-grade enamel coating, coated Stored in
(b) paperboard, and bag-in-box provide
Stored at a
the dark to
FFA Factor reduced
protection from light and oxygen. minimize
FFA factor = 1.7% (if FFA < 0.4%); 2.1% (if FFA > 0.4% Bag-in-box also has the advantage of
temperature
∘ light
and <0.6%); or 2.5% (if FFA > 0.6%): of 15 C [29]
maintaining minimum oxygen in exposure
17% − PPPs headspace [14]
(c) (11)
0.6%
This model recognizes that induction time generally cor- 2.10. Rodrigues et al. (2017) [38]. Coupled with powerful sta-
relates with olive oil FAPs and antioxidant content. DAGs tistical linear discriminant analysis (LDA) [49, 50] and sim-
and PPP have been shown to be predictable and change ulated annealing (SA) variable selection algorithm approach
linearly with time whereas FFA provides a value for the initial [51–53], a most recent study on the evaluation of EVOO shelf
oil quality and does not change significantly under proper life was conducted by applying a potentiometric electronic
storage conditions. These four quality parameters represent tongue (E-tongue) with nonspecific cross-sensitivity lipid
factors that can affect olive oil shelf life over time. membranes to assess the commercial storage conditions
To evaluate this empirical model, the research team including light exposure and storage time.
analyzed 118 samples for FFA, PV, UV, PPP, DAGs, and The research group had analyzed 36 amber glass-bottled
sensory evaluation during a 30-month storage period. The EVOO samples on sensory attributors (conducted by four
samples were stored in a dark environment at 18∘ C ± 2∘ C, trained panelists to classify samples based on olfactory sen-
and tested immediately after reaching their estimated best sations, gustatory-retronasal sensations, and final olfactory-
before date. Of the 118 samples, only one sample (0.8% of gustatory sensations), physicochemical parameters (FFA, UV,
total samples) exceeded the Australian limit of 0.8% for FFA; and PV) and oxidative stability (OSI), and electrochemical
no sample failed the Australian limit for PV (20 meq O2 /kg) signal profiles (E-tongue device with two print-screen poten-
or 𝐾232 (2.50 K1% 1 cm ); two samples (1.7%) failed 𝐾270 limit tiometric arrays containing 20 sensors on each one). To fur-
(0.22 K1% 1 cm ); twelve samples (10.2%) failed the Australian ther elucidate the sample storage and testing conditions, four
limit of 17% for PPP; six samples (5.1%) failed the Australian fresh samples were analyzed immediately after processing
limit of 35% for DAGs; and ten samples (8.5%) failed sensory at T0 (0 month) while 32 samples were kept under room
evaluation. In addition to testing 118 samples at the end of temperature (17–25∘ C) for one year in the lab, with 16 samples
shelf life under controlled storage condition, 20 samples with being stored in dark and 16 samples being exposed to natural
predicted shelf life were randomly collected from different light and artificial light (14 h/day from eight fluorescent
retailers every three months during a 30-month storage lamps) to create a 2 × 4 × 4 experimental factorial design.
period to validate the model from retailers’ standpoint (200 During the one-year storage period, four samples were taken
samples in total). Only one sample (0.5% out of 200 samples) out and analyzed every three months at time points of T3, T6,
exceeded the limit for 𝐾270 and two samples (1%) exceeded T9, and T12. As a result, the quality parameters and oxidative
the limit for DAGs at their predicted BBD. By recalculating stability of the tested EVOO samples were indeed affected by
and comparing the actual and predicted BBD, the data both the storage time and light conditions. It was inferred
suggested that producers may want to deduct 1-2 months by the authors that, being stored in amber bottles, light
from the BBD given from the model to compensate for the conditions played less significant role on the olive oil quality
potential exposure to heat and light during transportation, deterioration during the storage period. In addition, not all
handling, storage, and display on the retail shelves. the positive attributors of EVOO samples were affected by
This model was validated on a total of 318 samples, the storage conditions after one-year storage period, although
including 200 commercial samples from real-time storage samples exposed to light showed the strongest correlations
conditions on the market, with simple and straightforward among the respective sensory attributors (𝑅-Pearson ≥ 0.80).
calculations and yielded clear output. Modifications to the To evaluate the possibility of correctly categorizing olive
predicted BBD are necessary when storage condition is not oil samples based on storage time and/or light conditions
ideal; however, this would be true for any models that are (dark/light), the Kennard-Stone selection algorithm (a uni-
designed for the ideal packaging and storage conditions for form mapping algorithm that generates a flat distribution
olive oil shelf life (Table 9). of data suitable for regression model development) [56]
Journal of Food Quality 13

Table 10: Summary of statistical analysis performed by Rodrigues et al. (2017).

Statistical
Objective Statistical analysis∗
analysis ref.
Compare the impact of dark/light storage conditions on olive oils for each
Student’s 𝑡-test [48]
storage time
One-way ANOVA, Tukey’s post hoc
Assess the effect of the storage time on olive oils stored in dark/light [48]
multicomparison test
Evaluate the existence of bivariate correlations within the olive oil’s Linear Pearson correlation coefficient
[48]
physicochemical parameters (𝑅-Pearson)
Test the capability of the E-tongue to correctly classify the EVOO based on
storage time or storage conditions as a supervised pattern recognition Linear discriminant analysis (LDA) [49, 50]
method
Evaluate the qualitative classification capability of physicochemical and
LDA [49, 50]
sensory data
Select the best subsets of 𝐾 independent predictors among 40 E-tongue Metaheuristic simulated annealing (SA)
[51–53]
potentiometric signals variable selection algorithm
Compare the current and the new subsets of 𝑘 (⊆K) variables Tau2 quality criterion [51]
Evaluate the LDA classification models Leave-one-out cross-validation (LOO-CV) [54, 55]
24 olive oil samples used as “training set” for
Minimize the risk of overfitting from LOO-CV when sample size is large [54, 55]
LOO-CV
and generate a flat distribution of data for regression model development
12 olive oil samples used as “testing set” using
[56]
Kennard-Stone algorithm
∗
All statistical analyses were performed using Subselect [51, 57] and MASS [58] packages of the statistical program R (version 2.15.1) at a significant level of 5%.

was adopted by splitting 36 bottled olive oil samples into producer prices of EVOO have increased by more than 15%
two subsets (24 for internal validation and 12 for exter- (in euros) in Spain, Italy, Tunisia, and Greece compared to the
nal validation). By applying the metaheuristic SA variable same period in the previous year [61]. Thus, to maintain the
selection algorithm, the best subset to be included in each high quality of EVOO products during commercial activities
LDA model was selected from physicochemical parameters, has become an urgent matter to olive oil producers and being
sensory attributors, and E-tongue signal profiles for the deter- able to accurately predict the shelf life of EVOO products
mination of the effect of different storage conditions on the would greatly benefit both producers and consumers.
quality of EVOO samples. The internal validation statistical EVOO quality can be safeguarded by using proper pack-
data showed that E-tongue signal profiles yielded an over- aging, ideal storage conditions (cool and dark), and having
all better predictive discrimination performance, enabling an accurate best before date. Currently in literature, common
the establishment of three best LDA-SA prediction models parameters that are being used to track the changes in olive
(from 5 to 8 sensor/sensor-replicas as independent variables) oil include FFA, PV, UV, DAGs, PPP, sensory evaluation,
without redundant variables. The external validation further induction time, FAP, total tocopherols and total phenols, and
justified the predictive capability of E-tongue by giving a volatiles. A mathematical model for tracking deterioration
representative fingerprint of the polar compounds in olive oil using sensitive and accurate quality parameters can be a
samples. powerful and affordable tool for accurately predicting olive
As a promising chemometric approach, combining E- oil shelf life.
tongue measurement and comprehensive statistical analysis In this review, ten practical mathematical models that
(Table 10) could successfully determine the freshness of have potential to be adopted and utilized by olive oil pro-
EVOO samples during normal commercial storage condi- ducers are summarized. Nonetheless, each of the models can
tions (stored in dark or exposed to light for one year) benefit from further study with a large set of samples under
and provide accurate shelf-life prediction. Nonetheless, it is real-life transport and storage conditions, monitoring both
important and necessary that at least eight trained panelists compositional and environmental variables. To establish a
were presented to provide sensory data as the lack of sen- robust and systematic model for shelf life assessment, the
sory data could significantly influence the statistical analysis most urgent tasks are (1) to remove unnecessary parameters
results. and to confirm the acceptable limits without losing the
predictability and accuracy and (2) to continue developing
3. Conclusion and fine-tuning accelerated methods to minimize their ten-
dency for overprediction or underprediction of actual shelf
The global production and consumption of olive oil has life. By reducing inessential parameters used in a model,
escalated significantly in the past decade [60]. According to the processing time and cost of shelf life assessment are
the IOC Market Newsletter released in September, 2017, the also reduced. Since sensory evaluation remains to be one
14 Journal of Food Quality

of the most sensitive methods for olive oil quality and olive oil stability,” Journal of the Science of Food and Agriculture,
freshness, a working model should be calibrated with sensory vol. 85, no. 9, pp. 1492–1498, 2005.
evaluation and complement sensory evaluation for olive oil [11] A. Kiritsakis, G. D. Nanos, Z. Polymenopoulos, T. Thomai, and
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Conflicts of Interest packaging material headspace, oxygen and light transmission,
temperature and storage time on quality characteristics of extra
The authors declare that there are no conflicts of interest virgin olive oil,” Food Control, vol. 21, no. 4, pp. 412–418, 2010.
regarding the publication of this paper. [14] S. Wang, X. Li, R. Rodrigues, and D. Flynn, Packaging Influences
on Olive Oil Quality: A Review of The Literature, UC Davis Olive
Center, 2014.
Acknowledgments [15] X. Li, H. Zhu, C. F. Shoemaker, and S. C. Wang, “The effect of
This review was made possible with the financial support different cold storage conditions on the compositions of extra
virgin olive oil,” Journal of the American Oil Chemists’ Society,
from the Olive Oil Commission of California. The authors
vol. 91, no. 9, pp. 1559–1570, 2014.
would also like to thank Leandro Ravetti and Dan Flynn for
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helpful discussions.
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