Food Chemistry 141 (2013) 3827–3836

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Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Changes in nutritional and sensory properties of orange juice packed in

PET bottles: An experimental and modelling approach
Celine Bacigalupi a, Marie Hélène Lemaistre b, Naima Boutroy b, Christophe Bunel b, Stéphane Peyron a,
Valérie Guillard a, Pascale Chalier a,⇑
a
Joint Research Unit Agropolymers Engineering and Emerging Technologies-UMR 1208 Montpellier Supagro, INRA, UM2, CIRAD, CC 023, Pl. E. Bataillon, 34095 Montpellier
Cedex, France
b
Sidel, Octeville sur mer, BP 204, 76053 Le Havre Cedex, France

a r t i c l e i n f o a b s t r a c t

Article history: Sensitivity to oxidation of an orange juice was investigated through packaging in standard PET or active
Received 23 January 2013 PET with oxygen scavenger bottles. The evolution of dissolved oxygen was found to be similar in all bot-
Received in revised form 11 June 2013 tles, whereas ascorbic acid degradation was related to the oxygen transfer with higher losses in standard
Accepted 18 June 2013
PET (53%) against active PET (31%). Moreover, when juice was exposed to high intensity light, a fold faster
Available online 29 June 2013
degradation of ascorbic acid was observed compared to total darkness. Depending also on the light inten-
sity and regardless of the package permeability, changes in the aromatic profile of the juice were
Keywords:
observed due to the degradation of limonene and the formation of a-terpineol, an off-flavour. A mecha-
Packaging
PET
nistic model was developed to predict the shelf life of orange juice. This model, coupling O2 transfer and
Oxygen scavenger ascorbic acid oxidation reaction in the bottled juice, confirmed that oxygen permeation through packag-
Transfer ing material could not be neglected.
Ascorbic acid Ó 2013 Elsevier Ltd. All rights reserved.
Aroma compounds

1. Introduction
The sensory and nutritional properties of orange juice and con-
sequently its shelf life depend upon a large range of parameters re-
lated to the initial product quality, the conditions of processing and
the packaging properties (especially the ability of the packaging to
transmit O2 and light, both being involved in orange juice degrada-
tion). Vitamin C is degraded by oxidative and non-oxidative path-
ways, which results in both nutritional and organoleptic losses
(Yuan & Chen, 1998; Zerdin, Rooney, & Vermue, 2003). The two
pathways contribute to the formation of reductones, which are in-
volved in non-enzymatic browning reactions and lead to the for-
mation of volatile compounds, such as furfural (Kennedy, Rivera,
Lloyd, Warner, & Jumel, 1992; Rouseff, Nagy, Naim, & Zahavi,
1992), and brown pigments (Solomon, Svanberg, & Sahlström,
1995). Depending on the oxygen level, ascorbic acid degradation
would be a first-order reaction, with respect to ascorbic acid con-
centration (high oxygen level) or to oxygen (low oxygen level)
(Garcia-Torres, Ponagandla, Rouseff, Goodrich-Schneider, &
Reyes-De-Corcuera, 2009; Zerdin et al., 2003). However, at a lim-
ited level of dissolved oxygen, for instance, when different oxygen
barrier packagings were used, 2nd or zero-order kinetics were sug-
⇑ Corresponding author. Tel.: +33 467143891.
E-mail address: chalier@univ-montp2.fr (P. Chalier).
gested to describe the ascorbic acid oxidation (Polydera, Stoforos, &
Taoukis, 2003; Singh, Heldman, & Kirk, 1976). Recently, a linear
relationship was found between the first order ascorbic acid degra-
dation constants and the initial headspace oxygen concentrations
(Van Bree et al., 2012). It is obvious after analysis of the above-ci-
ted works that no clear consensus actually exists on the type of
equation to use to represent and model the vitamin C oxidation
in orange juice.
Changes in colour and in aroma profile induce depreciation of
sensory properties and the rejection of the orange juice by the con-
sumer. The colour change is due to the browning of the juice in
relation to Maillard reactions (Kacem, Cornell, Marshall, Shireman,
& Matthews, 1987; Solomon et al., 1995), and also to the isomeri-
sation and oxidation of carotenoids, which are influenced by heat,
light and oxygen (Baker & Gunter, 2004).
Although limonene is the aroma compound that displays the
highest concentration in orange juice (50–130 ppm), the aroma
profile of orange juice is largely determined by compounds present
at concentrations of less than 1 ppm such as terpenes or terpenols,
aldehydes or esters (Averbeck & Schieberle, 2009; Perez-Cacho &
Rouseff, 2008). The aromatic profile of orange juice can be modified
by the formation of new compounds, through oxidation or acid-
catalysed reactions (Clark & Chamblee, 1992; Perez-Cacho &
Rouseff, 2008). For instance a-terpineol, which has a stale, musty
or pine-like off-flavour, is formed from the degradation of both

0308-8146/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.foodchem.2013.06.076
3828 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836
limonene and linalool (Haleva-Toledo, Naim, Zehavi, & Roussef,
1999).
Oxygen strongly affects all the aforementioned reactions (Kene-
dy et al. (1992), Perez-Cacho and Rouseff (2008), Petersen, Tonder,
and Poll (1998), Polydera, Stoforos, and Taoukis (2005), Solomon
et al. (1995)). Oxygen is present during bottling as dissolved O2
in the juice and gaseous O2 in the headspace but also diffuses from
the surrounding atmosphere through the packaging material into
the juice with a rate depending on the permeability of the material
and the difference in O2 partial pressure on both sides of the pack-
aging. Adequate sizing of O2 permeability of the packaging mate-
rial can increase the shelf life of the juice by avoiding oxidative
degradation. In this sense, high barrier materials are usually se-
lected, such as glass bottles, foil laminates in carton packs (e.g.,
Tetrapak) or flexible pouches and polyethylene terephthalate bot-
tles (PET) (Berlinet, Brat, Brillouet, & Ducret, 2006; Kennedy et al.,
1992; Petersen et al., 1998; Polydera et al., 2003). PET is increas-
ingly used in beverage packaging, due to its excellent mechanical
properties, UV resistance and good oxygen barrier properties,
which can be improved by combining different films (multilayer
PET) or by adding oxygen scavengers to monolayer or multilayer
PET (Berlinet, Brat, & Ducret, 2008; Ros-Chumilla, Belissario, Iguaz,
& Lopez, 2007; Zerdin et al., 2003). In these active packages, scav-
engers act by reducing the oxygen content dissolved in the juice
and present in the headspace but also by limiting oxygen ingress
and increasing the shelf life.
Besides oxygen, temperature and light strongly affect the reac-
tion phenomena by activating diffusion and reaction rates. The ef-
fect of light exposure (fluorescence, UV) on orange juice quality has
not been much investigated and findings on vitamin C are often
contradictory (Conrad, Davidson, Mulholland, Britt, & Yada, 2005;
Solomon et al., 1995). Its effect depends on the nature and the
intensity of light and on the UV barrier properties of packaging
but also on the nature of the juice. Conrad et al. (2005) showed that
ascorbic acid degradation was dependent on light in apple juice
but not in orange juice. Berlinet et al. (2008) did not observe any
effect of artificial light on the vitamin C content of a juice whatever
the type of packaging material (standard PET or multilayer PET
with oxygen scavenger), probably because both materials display
similar UV transmission properties.
Numerous studies can be found dealing with the nutritional and
sensory quality of orange juice. However, as far as we know, no
study has yet considered oxidation of vitamin C and changes in ar-
oma profile with variation in dissolved oxygen and oxygen barrier
properties, and the effect of light exposure. Moreover, to rationally
design orange juice packaging, it is necessary to quantitatively
evaluate the influence of the oxygen content within the juice and
the impact of oxygen ingress in the bottle on the oxidation kinetics.
Upto now, dimensioning of O2 barrier properties of packaging
material is done empirically with a ‘‘pack-and-pray’’ approach,
which is expensive and time-consuming, due to the long shelf life
of pasteurised orange juice (>6 months). An alternative would be to
propose a mathematical model coupling O2 transfer and oxidation
reactions in the bottle, permitting the prediction of the shelf life of
the juice on the basis of ascorbic acid losses and to identify the O2
permeability that best suits the target product.
The objectives of this study were to evaluate the ascorbic acid
content and the change in aroma profile of an orange juice packed
in different lightweight PET-based bottles. We used a standard PET
vs. two PETs with oxygen scavengers during 6 months of storage at
three different light exposures. Changes in nutritional and sensory
properties of the juice were related to O2 content in the bottle, O2
barrier properties of the packaging and light exposure. These re-
sults were then used to tentatively validate a mathematical model
aiming at predicting evolution of orange juice quality during
storage.
2. Material and method
2.1. Reagents
Analytical metaphosphoric acid (33.5–36.5%), 2,6-dichlorophe-
nolindophenol sodium salt hydrate (purity P 97%, based on dry
substance), sodium bicarbonate (purity P 99.7%), ferric chloride
hexahydrate (98–102%) and ascorbic acid (purity P 99.0%) were
supplied by Fluka.
Glacial acetic acid (99–100%), absolute ethanol (analytic grade),
orthophenanthroline (99%) and ammonium acetate (purity P 98%)
were obtained from Sigma–Aldrich, as well as aroma compounds
limonene, linalool, b-myrcene, a-pinene, furfural, limonene oxide,
carvone and 2-heptanol (purity > 99%).
2.2. Packaging material
Three PET grades were used in this study: a standard monolayer
PET and two active monolayer PETs including an oxygen absorber,
called PETOS1 and PETOS2 and provided by two different suppliers.
Standard PET can be considered as a passive package compared to
the active packages containing oxygen absorbers. Preforms were
kindly blow-moulded by Sidel (Le Havre, France) to obtain bottles
with 25-cl capacity, weighing 14 g. The thickness of the bottles
(measured at body level) was 150 lm (±1.5). All bottles were
closed using polyethylene caps without any internal joint supplied
by Bericap (Longvic, France).
2.3. Preparation of orange juice from concentrate and conditioning
Concentrated orange juice (65° Brix) was supplied by LSDH (Lai-
terie de Saint Denis de l’Hôtel, France). Sidel prepared the juice and
filled the bottles using pilot machines. The concentrated juice was
diluted in a tank by adding water under agitation (600 rpm) to ob-
tain a ° Brix of 11.6. The juice was degassed at 65 °C under vacuum
(0.65 mbar) and then flash pasteurised for 20 s at 95 °C in the
pasteurisation pilot (Sidel, Le Havre, France). The juice was cooled
to 20 °C and maintained in a sterile tank before filling at 5 °C and
under 130 mbar of pressure to avoid microbial contamination.
Then, the orange juice was packed in the three different PET bottles
using a semi-automatic filler (Sidel, Le Havre, France). Bottles were
previously sterilised by injection of peracetic solution (1800 ppm)
for 10 min, under a pressure of 2 bars at 54 °C and the caps were
treated by ionisation. Before filling, the bottles were washed with
sterilised water previously filtered through a 0.45-lm membrane.
After filling, the headspace was renewed under N2 flux at 1 bar and
the bottles were manually closed with the caps. To verify the effi-
ciency of pasteurisation and filling, microbial analyses were carried
out by enumeration of total flora on PCA (mesophilic and anaero-
bic) and evaluation of mould contamination on PDA.
The samples packed in standard PET bottles were stored at
22 ± 0.5 °C in total darkness or under white light with a radian flux
of 400 lux (40 W, 4000 K, 3200 lumens) or of 10,000 lux (150 W,
6000 K, 11,250 lumens) (S.B.F, France). The samples packed in
PET with oxygen absorbers were stored at only 400 lux.
2.4. Methods
Analyses were carried out at different times: 0, 7, 15, 22, 30, 60,
90, 120, 150 and 180 days and performed in triplicate with 3 differ-
ent bottles under each condition or packaging.
2.4.1. Oxygen transfer rate (OTR)
The oxygen transfer rate was measured on a MOCON OX-TRAN
2/20 instrument (MOCON, Minneapolis, MN) according to the
 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836
ASTDM-D3985 standard method. It is a steady state, isostatic
method using a coulometric sensor. The test specimen was held
so that the two sides of a test chamber were separated: one side
was exposed to nitrogen and the other to air (i.e. O2 at 21%). The
temperature was maintained at 23 °C and the relative humidity
at 50% whatever the test specimen (passive or active packaging).
OTR was measured at to and after 1, 3 and 6 months of storage be-
cause the efficiency of active packaging can vary according to the
capacity of the absorbers. Each test trial consisted of 5 replicates.
2.4.2. Measurement of local O2 content in juice
Local oxygen partial pressure was determined using a Fibox 3
fibre optic oxygen meter purchased from PreSens Precision Sensing
GmbH (Neuburg, Germany).
The O2-sensitive optical sensors (spots of 4 mm diameter) se-
lected for this study were the PSt3 sensors (PreSens Precision Sens-
ing GmbH) that can be used for a range of oxygen pressures
ranging from 0% to 100% O2 (with a limit of detection at 0.03%
and an accuracy of ±0.4% O2 at 20.9% O2 and ±0.05% O2 at 0.2%
O2). A conventional two-point calibration in an oxygen-free envi-
ronment (nitrogen or sodium sulfite), and saturated air environ-
ment (i.e. 21% O2) was performed before use. A PSt3 sensor was
glued inside each bottle, using silicone glue, prior to closure. The
dot was located in the orange juice about 2 cm below the neck.
We measured dissolved O2 just at the interface between the bottle
material and the juice. The interest of this local non-invasive mea-
surement was that it avoided modifying the diffusion rate of O2
within the juice by shaking the bottle to homogenise the O2 con-
tent before the measurement. The optical fibre which was con-
nected to the oxygen transmitter was placed on the outer surface
of the bottle, right opposite the sensor spot and emitted an excita-
tion light through the wall. Data acquisition was performed using
PST3 software (PreSens – Precision Sensing GmbH, Regensburg,
Germany). For each measurement, the temperature was fixed at
20 °C, and the oxygen measurements were compensated accord-
ingly. This method proved to be very efficient for monitoring O2 in-
gress in wine bottles during storage (Dieval, Vidal, & Olav, 2011).
2.4.3. Ascorbic acid analysis
Ascorbic acid contents of orange juice were measured by a
method previously developed by Pénicaud, Peyron, Bohuon, Gon-
tard, and Guillard (2010), and based on redox reaction between
ascorbic acid and Fe (III), monitored by spectrophotometry at
505 nm and using microplates. Vitamin C was extracted with aque-
ous metaphosphoric acid 3% – acetic acid 8% solution, as recom-
mended in the official method (AOAC, 2007). In short, the
extracted sample or fresh standard solutions (15 ll) were spread
out into a wells plate and reacted with 50 ll iron (III). The covered
plate was stored for 10 min at room temperature before the addi-
tion of orthophenanthroline (50 ll) then incubated for 15 min at
room temperature. Finally, ammonium acetate was added: 135 ll
in the measurement wells, 185 ll in the blank wells. The plate
was incubated for 2 h at room temperature, and absorbences were
read at 505 nm using a microplate reader (Multiskan Spectrum,
Thermo Electron Corporation, Saint-Herblain, France). A standard
curve could be obtained from the standard solutions values, and
from these data all well concentrations could be obtained. Each
analysis was performed in triplicate on three different bottles from
the same storage time and condition. The limit of detection of this
method at 95% confidence level was found to be equal to 11 mg l1
by Pénicaud, Guilbert, Peyron, Gontard, and Guillard (2010) and
the limit of quantification at the same confidence level of
21 mg l1.
3829
2.4.4. Extraction of aroma compounds of orange juice
Fifty millilitres of orange juice (containing 200 ll of 2-heptanol
solution at 50 mg/100 ml of ethanol used as internal standard)
were extracted with 2  50 ml of dichloromethane forduring 30
and 15 min under 500 rpm agitation at ambient temperature. After
each homogenisation, the resulting emulsion was disrupted by
freezing for 2 h at 18 °C. The organic and aqueous phase were
separated by decantation and gathered before being dried on anhy-
drous sodium sulfate and concentrated under nitrogen flux to a fi-
nal volume of 1 ml.
2.4.5. Quantification of aroma compounds by GC-FID analysis
GC-FID analysis was performed for the quantification of the ar-
oma compounds. A Varian 3800 GC equipped with an automatic
sampler (Combipal; CTC, Zwingen, Switzerland), a DB-WaxÒ col-
umn (30 m  0.25 mm, film thickness of 0.25 lm; J & W Scientific,
Folsom, CA) and a flame ionisation detector (FID; hydrogen,
30 mL min1; nitrogen, 30 mL min1; air, 300 ml min1) was used.
Hydrogen was the carrier gas at a flow rate of 1.5 ml min1. The
temperature was set at 250 °C for the injector and 300 °C for the
detector. Programmed thermal conditions were used: oven tem-
perature initially at 40 °C was maintained 3 min, then raised by
3 °C min1 to 250 °C, and was kept at 250 °C for 10 min. Selected
aroma compounds were identified using known standards and
the quantification was performed using the internal standard for
which the response coefficient of each compound was determined.
2.4.6. Identification of aroma compounds by GC/MS analysis
An Agilent 5973 series gas chromatograph equipped with an
autosampler (Combipal; CTC) and a DB-WaxÒ analytical fused-sil-
ica column (30 m  0.25 mm  0.25 lm film thickness; J & W Sci-
entific) and coupled with a 5989A quadrupole mass spectrometer
in electron ionisation mode, was used for identification. The elec-
tron impact (EI) energy was 70 eV and the quadrupole temperature
was set at 250 °C. The injector was heated at 250 °C and used in
split mode (20:1). The oven temperature was held at 40 °C for
5 min, ramped to 250 °C at a rate of 4 °C/min and maintained at
250 °C for 10 min. The carrier gas was Helium 6.0 (Air Products,
Basingstoke, UK), with a flow-rate of 1.5 ml/min. The detection
was carried out in full scan mode covering a mass range (m/z) of
50–450 amu. The aroma compounds were identified from their
mass spectra using the Wiley 275.L library (Agilent Technologies).
Attribution was performed on peaks showing a signal to noise S/
N > 3 and identification of the compound was valid when the con-
fidence rating of mass spectral comparison was superior or equal
to 95. This attribution was further confirmed using relative reten-
tion indices and by injection of reference compounds. A standard
solution of alkanes (C11 to C27) was analysed by GC/MS using the
same GC conditions to calculate linear retention indices (ITs ).
2.5. Statistical analyses
Statistical analyses were performed to examine the effect of
packaging and storage conditions on vitamin C content and aroma
compounds. Significant differences between samples were esti-
mated by analysis of variance (ANOVA). The statistical significance
level was set to 0.05. Statistical analyses were performed using R
software (free access, http://www.r-project.org/).
3. Results and discussion
The orange juice was packed in monolayer passive PET bottles
(standard PET) and in active PET containing oxygen scavengers
(PETOS1 and PETOS2). All bottles were stored at 20 °C (±2 °C)
and 400 (±5) lux to imitate the conditions of conventional shelf
3830 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836
storage. To evaluate the effect of light, orange juice packed in stan-
dard PET bottles was stored at 20 °C in the dark and at 400 and
10,000 lux.
3.1. OTR evolution of PETs during storage
The oxygen transfer rate (OTR) of each material (standard PET,
PETOS1 and PETOS2) was measured just before filling and after dif-
ferent storage times (0, 1, 3 and 6 months) at 20 °C and 400 lux, in
order to verify that the bottles maintained or not their oxygen bar-
rier properties until the end of shelf life (6 months). As expected,
both active PET (PETOS1 and PETOS2) showed very low initial OTR
(i.e. at time 0 before filling), since the value was below the detection
limit of the method (0.0005 ± 0.0000), confirming the role of the
oxygen scavenger in both cases. In contrast an OTR equal to
0.0291 ± 0.0005 cc bottle1 day1 was measured for standard PET
and remained unchanged during the 6 months of storage. For both
active PETs, as expected, OTR strongly increased, to 0.0041 ±
0.0010 cc bottle1 day1 for PETOS1 and 0.0035 ± 0.008 cc bot-
tle1 day1 for PETOS2 (up to 8 times) after 3 months of storage.
Accordingly, active PETs lost a part of their initial barrier capacity
after 3 months of storage but remained more effective than standard
PET. It was obvious from these OTR data that oxidation phenomena
would be more pronounced in standard PET than in active PET.
3.2. Evolution of dissolved oxygen content in orange juice during
storage
After filling, the initial concentration of dissolved oxygen in
juice was around 0.98 ± 0.17 ppm (or mg l1). It is important to
note that for t > 0 the measurement of O2 content was representa-
tive of the local concentration around the dot stuck at 2 cm below
the neck, i.e. very close to the juice/headspace interface, and on the
internal face of the bottle. Whatever the package and light inten-
sity, the local oxygen content decreased dramatically during the
first days of storage to reach 0.12 ppm (Fig. 1). When the bottles
were stored at 400 lux, the values of local dissolved oxygen were
stable from the 15th day up to the 90th day and then began to in-
crease. After 6 months of storage, no significant differences were
1.20
1.00
0.80
O2 in ppm
0.60
0.40
0.20
0.00
0 30
Fig. 1. Evolution of dissolved oxygen in orange juice packed in standard PET bottle and stored in total darkness (), at 400 lux ( ), at 10,000 lux (j) and at 20 °C or in PET
bottles with oxygen scavengers PETOS1 ( ) PETOS2 (D) and stored at 400 lux and at 20 °C.
observed between the three PETs despite their varying barrier
properties. A concentration of oxygen around 0.37 ± 0.09 ppm
was obtained for all the stored bottles at 400 lux at the end of
the storage, whatever the type of PET. The initial decrease of dis-
solved oxygen would be due to its consumption by oxidative com-
ponents, such as vitamin C and aroma compounds, whereas the
further increase could be explained by a higher O2 ingress via the
packaging rather than its consumption by reactions (Garcıa-Torres,
Ponagandla, Rouseff, Goodrich-Schneider, & Reyes-De-Corcuera,
2009). Variations in OTR values between passive (standard) and ac-
tive (oxygen scavenger) PETs (i.e. 8–9 times lower for active pack-
aging than for standard PET) did not affect the concentration of
local oxygen content in the orange juice. We noted that the posi-
tion of the dot in the bottle may vary from one bottle to another,
leading to difficulty in comparison between PETs. Because of this,
we cannot make a conclusion about the average amount of O2 in
the juice, which could differ between PET types
In contrast, changes in light intensity during storage clearly af-
fected the dissolved oxygen concentration, since in total darkness,
the dissolved oxygen was stable throughout the storage but in-
creased at 400 lux and at 10,000 lux. At 6 months of storage, dis-
solved oxygen was significantly different for the three conditions.
This could be explained by a modification of OTR with light, due
to the photosensitivity of PET combined with the possible oxida-
tion of the cap composed of polyethylene.
3.3. Changes in concentration of ascorbic acid during storage
The concentration of ascorbic acid was monitored during the
storage of orange juice at 20 °C in different packages and light con-
ditions (Fig. 2). The initial ascorbic acid content just after packag-
ing was found to be 521 ± 7 mg l1. Whatever the package and
the light conditions, a large decrease in ascorbic acid (25–34% of
initial content) was observed from the beginning of the storage
to day 30 (Fig. 2). This trend coincided with the steep decrease of
dissolved oxygen in the juice (Fig. 1) and can be attributed to the
consumption of oxygen initially present in the bottle, i.e. dissolved
in the juice and present in the headspace. After the first month, the
loss of ascorbic acid was more gradual as shown by other studies
60 90 120 150 180
time (day)
 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836
Fig. 2. Changes in ascorbic content of orange juice packed in standard PET bottles stored in darkness (), at 400 lux ( ), at10,000 lux (j) and at 20 °C or in PET bottles with
oxygen scavengers PETOS1 ( ) and PETOS2 (D) and stored at 400 lux and at 20 °C.
(Berlinet et al., 2006; Kennedy et al., 1992; Zerdin et al., 2003). Up
to 90 days, ascorbic acid oxidation seemed independent of the oxy-
gen barrier properties of the packages, whereas, after this duration,
significant high losses of ascorbic acid were found for juice packed
in standard PET bottles compared to active PET bottles. Using stan-
dard PET, the ascorbic acid degradation was worse and losses
reached 53% of the initial quantity at 6 months of storage, whereas
losses were 41% and 31% at the end of storage for PETOS1 and PE-
TOS2, respectively. At this time, the OTR of standard PET was 8-fold
higher than those of both active PET bottles, leading to higher
transfer of oxygen and probably greater losses of ascorbic acid
through oxidation. The OTR difference between the two PETOS
did not significantly impact the ascorbic losses, except after
6 months of storage. At this time, the more efficient active PET (PE-
TOS1) led to a reduction in losses of 25%.
The interest of O2 scavengers for preserving vitamin C from oxi-
dation in orange juice had already been pointed out in the litera-
ture. Indeed, Berlinet et al. (2006) found that the losses of
ascorbic acid in an orange juice packed in a 0.33-l monolayer PET
bottle and a multilayer PET bottle containing an oxygen scavenger
during 6 months of storage at 20 °C and under artificial light with
an intensity of 750 lux reached 60% and 30%, respectively. Simi-
larly, Ros-Chumilla et al. (2007) reported higher losses of vitamin
C in orange juice packed at 25 °C in darkness with standard PET
(1-l bottle) than with active PET.
Concerning the light conditions of storage, no significant differ-
ences were observed between 400 lux and darkness for orange
juice packed in standard PET, whereas a significantly higher degra-
dation of ascorbic acid was highlighted from 3 months of storage at
10,000 lux (Fig. 2). After 6 months of storage, 64% of ascorbic acid
was lost against 53% for both other conditions (400 lux and dark-
ness). This result was at variance with previous studies performed
using lower light intensities (1500–2000 lux), which emphasised
no light effect on ascorbic acid losses in PET bottles (Berlinet
et al., 2008; Conrad et al., 2005) or other material (Solomon
et al., 1995). Two hypotheses may be expressed to explain higher
losses of ascorbic acid obtained under the strong light conditions
(10,000 lux) used in our study. First, it may be suggested that the
accelerated degradation of ascorbic acid is related to the strong in-
gress of oxygen observed for this storage condition (Fig. 1). Second,
a light-induced degradation of ascorbic acid may occur in addition
to the auto-oxidation phenomenon that would provoke an appar-
3831
ent increase in ascorbic acid degradation rate. Currently, according
to the scientific literature data, there is no evidence of an effect of a
high level of light (>1000 lux) on the degradation of ascorbic acid.
The shelf life of orange juice is usually estimated from the vita-
min C concentration at the end of storage, a value higher than
200 mg l1 at the end of shelf life being recommended by AIJN
(2005). Our results showed that with both active PET in all condi-
tions of light exposure and with standard PET (for light exposure
<400 lux), the vitamin C content was greater than 200 mg l1, i.e.
314, 370 and 250 mg l1, respectively. In contrast, the juice stored
at 10,000 lux in standard PET contained only 195 mg l1 of ascorbic
acid after 6 months and consequently was no longer saleable.
3.4. Evolution of aroma compounds during storage
GC–MS analysis of the orange juice aroma compounds allowed
us to identify 25 compounds including 12 terpenes and sesquiter-
penes, 6 terpenols, 1 aliphatic alcohol, 1 ester, 1 acid, 2 ketones and
2 aldehydes (Table 1). Quantification showed that limonene (citrus
aroma) was the major compound (54.3 ± 1.4 mg l1) followed by b-
myrcene, a-pinene, valencene, linalool, a-terpineol and terpinen-
4-ol. The other compounds were present below 0.1 mg/l.
Limonene, linalool (floral) a-pinene and b-myrcene, identified as
key odorants of orange juice (Averbeck & Schieberle, 2009), were
present in concentrations above their odour thresholds determined
in water (34, 0.22, 5 and 14 lg l1, respectively). Their odour
activity values, OAV, calculated by dividing the concentration of
odorant by the odour threshold, reached 1597, 4545, 200 and 80,
respectively, confirming their odorant impact Ahmed, Dennison,
Dougherty & Shaw (1978).
Only certain compounds were quantified during storage: those
susceptible to degradation (limonene, linalool), those formed as a
result of degradation (limonene oxide, carvone, cis and trans-carve-
ol, a-terpineol, terpinen-4-ol and furfural), and those with an odor-
ant impact (a-pinene, b-myrcene). Whatever the packaging type,
the limonene level decrease was similar, with a faster degradation
during the first month than the following 5 months (Fig. 3). No sig-
nificant differences were observed between passive and active PET.
Losses of limonene reached 50% of the initial quantity (i.e.
28 mg l1) after 6 months of storage at 20 °C and 400 lux or in
darkness using the different PETs. Berlinet, Ducret, Brillouet, and
Brat (2005) only reported 30% of losses, i.e. 40 mg l1 of losses,
3832 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836

Table 1 sorial quality of juice. However, as for limonene, the degradation of

Volatile flavour components of orange juice just after filling (t = 0) these monoterpenes could not be related to the content and trans-
Component IR lita IR GC–MSb Concentration mg l1 fer of oxygen, since no significant differences were observed be-
a-Pinene 1038–1039 1029 1.06 ± 0.07 tween different packagings. It can be also suggested that the
Ethyl butanoate 1048–1040 1050 0.09 ± 0.03 effect of oxygen would be masked by acid-catalysed reaction (Per-
d-Carene 1148 1132 tr ez-Cacho & Rouseff, 2008). Accordingly, it was shown that oxygen
b-Myrcene 1148 1151 1.13 ± 0.14 removal did not improve the sensory properties of orange juice
Limonene 1192–1183 1185 54.26 ± 1.38
c-Terpinene 1224–1251 1228 0.07 ± 0.01
stored for 5 months (Trammell, Dalsis, & Malone, 1986). On the
p-Cymène 1261 1254 tr other hand, these compounds showed a great reactivity under
a-Terpinolene 1264–1284 1240 tr strong light, which could be associated with the formation of oxi-
Octanal 1267–1276 1268 tr dation products caused by allylic oxidation (Nguyen et al., 2009).
Hexanol (IS) 1351–1392 1361
The higher reactivity of b-myrcene relative to limonene or a-
Furfural 1432–1455 1450 tr
a-Copaene 1488 1464 0.10 ± 0.03 pinene could be associated with greater allylic hydrogen. It would
Linalool 1525–1537 1534 0.96 ± 0.06 have been of interest to study the effect of strong light in the pres-
Octanol 1537–1566 1542 0.08 ± 0.01 ence of oxygen absorbers.
b-Cubebene 1546 1560 0.10 ± 0.04 Linalool was degraded during storage and no difference was ob-
b-Caryophyllene 1562–1594 1565 0.15 ± 0.04
served between the different PETs. However, in contrast to terp-
1-terpine-4-ol 1591 1580 0.19 ± 0.02
b-Terpineol 1616 1605 tr enes, no significant effect of light was observed (Fig. 3). After
Sesquiterpene nd 1659 0.09 ± 0.01 6 months, losses reached 40% of the initial quantity of linalool. A
a-Terpineol 1688 1676 0.16 ± 0.04 more drastic decrease (49%) was observed by Berlinet et al.
Valencene 1751 1687 0.91 ± 0.13
(2005) after only 5 months using a multilayer PET with a 2-fold
Carvone 1720 1704 0.09 ± 0.01
Trans carveol 1801 1813 0.08 ± 0.02 higher initial concentration of linalool. In agreement with our re-
Cis carveol 1820 1801 tr sults, the final concentration of aroma compounds varied between
Hexanoic acid 1829 1829 0.10 ± 0.01 6% and 38% of the initial level after 12 weeks of storage for orange
Nootkatone 2250–2366 2473 tr juices obtained by high pressure or thermal treatment and condi-
tr trace (<0.05 mg/l), IS (internal standard). tioned in PET bottles and stored at 4 or 10 °C (Baxter, Easton, Sch-
a T
Is litterature : linear retention index were extracted from http://www.phero- neebeli, & Whitfield, 2005).
base.com/database/kovats or from Berlinet et al. (2005). a-Terpineol is a derivate of linalool and limonene. It was ini-
b T
Is calculated linear retention index from GC data.
tially present at a very low amount (0.16 ± 0.04 mg l1) but as ex-
pected, its concentration increased during storage for all the
different packages and storage conditions. After 6 months, an 8-
for orange juice packed in a monolayer PET and stored 5 months at fold increase was observed. In their study, Berlinet et al. (2005) ob-
20 °C in total darkness for a higher initial amount of limonene served only a 4-fold increase regardless of the packaging material
(130 mg/l). However, it was difficult to make a comparison with employed. It can be noted that the initial concentration was higher
the Berlinet et al. study, due to the different concentrations of lim- than in our study, probably due to its formation during processing.
onene, as well as there being no data regarding oxygen concentra- The detection threshold of this aroma compound imparting a stale,
tion. For orange juice stored at 10,000 lux, significant difference in musty or pine-like, odour is 2.5 ppm. After 6 months of storage, the
limonene content was observed from 2 months onwards. At the concentration largely remained below this value. Linalool is a more
end of storage, 65% of limonene was lost, i.e. more than 10 mg l1, reactive substrate than limonene for producing a-terpineol. How-
compared to the other conditions. ever, since there is more limonene than linalool in citrus juices,
It was observed that limonene could be rapidly degraded under a-terpineol appeared to be formed from both precursors (Haleva-
UV irradiation (48 h at 37 °C) resulting in the formation of a mix- Toledo et al., 1999). Regarding terpinen-4-ol, generated from a-
ture of products and a caraway-like and minty odour (Nguyen, pinene and limonene, no increase was observed during storage.
Campi, Jackson, & Patti, 2009), due to carvone enantiomers (Aver- Furfural, which can be formed from ascorbic acid decomposition,
beck & Schieberle, 2009). The carvone concentration was about was initially present (Table 1) but its quantification was possible
0.02 ± 0.01 mg l1 at 22 days, regardless of the storage conditions only after 7 days of storage. Its concentration slightly increased
and PET used, except at 10,000 lux (Fig. 3). In this case, the forma- up to 0.2 mg l1 whatever the packaging and the storage condi-
tion of carvone was 10 times higher (0.18 mg l1) at 22 days of tions. Its formation was not perturbed by the rate of ascorbic acid
storage and then decreased to reach 0.04 mg l1 at 3 months. We degradation depending on oxygen barrier properties of the packag-
can conclude that carvone formation is increased by intensive ing. However, it is an intermediate product, which can be also de-
light, which is in agreement with the high rate of carvone observed graded as quickly as it is formed.
when limonene was submitted to UV light (Nguyen et al., 2009). In short, for the 10 aroma compounds studied here, no signifi-
Among the other limonene degradation products, the presence cant differences were noticed in their degradation during storage
of limonene oxides and carveol was not evidenced during the en- of the juice in different barrier PET bottles. No impact of packaging
tire storage time. The limonene oxides and carvone were formed type on oxygen level was observed in agreement with the results of
in parallel but oxides have a relatively faster rate of formation than Berlinet et al. (2005), who highlighted that changes in aromatic
carvone (Haleva-Toledo et al., 1999). Moreover, limonene oxides profile of orange juice are independent of the oxygen permeability
can be converted into other products faster than they are formed. of the PET material. The main degradation pathways of aroma com-
Regarding the two other monoterpenes, a-pinene (pine-tree- pounds are probably due to acid catalysed reactions as well as to
like smell) and b-myrcene (geranium-like odour), a strong decrease aroma sorption in PET (Berlinet et al., 2005). However, a high level
in concentration was observed : the losses reached Fig. 3 100% and of light induced more drastic degradation and the formation of a
51%, respectively for all the juices stored in dark or at 400 lux. Un- higher amount of carvone, one of the oxidation products of limo-
der 10,000 lux, the degradation of the two compounds was acceler- nene. With regard to the losses of key aroma compounds, which
ated and 84% loss was noticed for b-myrcene after 6 months of can reach up to 40–100%, OAV were strongly decreased but they
storage. They are minor components but they contribute signifi- remained higher than 1, except for a-pinene (pine odour), which
cantly to the flavour and their losses can negatively affect the sen- was not detected after 6 months of storage. From this study, it is
 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836 3833

Fig. 3. Evolution of limonene, b-myrcene, a-pinene, linalool and a-terpineol in orange juice packed in standard PET bottles and stored in total darkness (), at 400 lux ( ), at
10,000 lux(j) and at 20 °C or in PET bottles with oxygen scavengers PETOS1 ( ),PETOS2 (D) stored at 400 lux and at 20 °C.

supposed that limited changes occur to the sensorial properties of
the juice. Moreover the fast and continuous oxidation of ascorbic
acid led to a reduced content of oxygen and reactive oxygen spe-
cies and thus protected the aromatic profile against oxidation.
3.5. Modelling the shelf life of bottled orange juice
The experimental results previously presented confirm that
ascorbic acid losses can be rightly considered as a marker of the
sensitivity of a product to the level of oxygen and thus the evolu-
tion of quality of orange juice during storage. The possibility to pre-
dict in advance ascorbic acid losses during storage of a packed
orange juice would be very helpful to allow a correct design and
sizing of the packaging material. In order to develop such a tool,
a mechanistic model previously developed by Pénicaud, Broyart,
Peyron, Gontard, and Guillard (2011), coupling O2 transfer (Fick’s
model) and ascorbic acid oxidation reaction, was upgraded and
adapted to the present study. These authors used Eq. (1) as the oxi-
dation model.
tial order of reactions with respect to ascorbic acid and dissolved
oxygen. In Eq. (1), the impact of both O2 and ascorbic acid content
(affected by partial order of reaction) on the reaction rate are taken
into account, which is rare compared to all the previous studies car-
ried out on the oxidation kinetic of ascorbic acid. Indeed, ascorbic
acid oxidation has been often described using first order kinetics,
with respect to AA concentration or zero order reaction (Conrad
et al., 2005; Garcia-Torres et al., 2009; Polydera et al., 2003; Zedin
et al., 2003). By using Eq. (1), a direct coupling of a mathematical
model for O2 diffusion with AA oxidation equation could be made:
the concentrations of O2 at time t in the product being one of the
outputs of the diffusion model (Fick’s model) and one of the inputs
required in Eq. (1).
In the present work, the model of Pénicaud et al. (2011) was up-
dated in order to take into account O2 ingress into the bottle
through the packaging material, which was represented as follows:
dO2 P
¼ AðpO2 outside  S  O2d Þ ð2Þ
dt e

r AA ¼ k½AAa ½O2 b ð1Þ where P, e and A are, respectively, the permeability, thickness and
surface of the packaging material, pO2 outside is the external partial
where AA and O2 represent ascorbic acid and dissolved oxygen con- pressure of O2, S is the solubility of O2 in the juice and O2d is the
tent (mol l1) in food, k is the kinetics constant rate, a and b are par- concentration of dissolved oxygen at time t. Then at the interface
3834 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836

Fig. 4. Description of the food/packaging system considered in the modelling approach.

Table 2
Input parameters required for predicting average concentration in ascorbic acid (AA) and dissolved O2 as a function of time during storage of orange juice at 20 °C and 400 lux.

Geometry of the system Diffusion model Reaction model

Bottle thickness 370  106a O2 solubility (mol l1 Pa1) 1.35  108b k (mol1.2 l1.2 s1) 3.0  102b
(m)
Bottle surface (m2) 26050  106 O2 diffusivity in juice 0.31  109b a (–) 1b
(m2 s1)
Headspace volume 17 AA diffusivity in juice 2.26  109b b (–) 1.2b
(mL) (m2 s1)b
Bottle width (mm) 160 O2 diffusivity in headspace 16  106c Initial O2 concentration in juice 0.98
(m2 s1) (mg l1) (±0.17)
Juice volume (mL) 250 Permeability 9.015  1018 for passive PET 1.308  1018 for Initial AA concentration in juice 521 (±7.1)
(mol m1 s1 Pa1) active PETOS1 (mg l1)
External O2 partial pressure 21,273 Initial O2 concentration in 21
(Pa) headspace (%)

Other parameters are from this study.

a
Supposed to be homogeneous. This average thickness taking into account the neck was calculated from the thickness profile of the bottle obtained from Sidel.
b
From Pénicaud et al. (2011).
c
From Sidel.

headspace/juice, O2 was assumed to be dissolved according to
Henry’s law (see Table 2 for the model parameters and Fig. 4 for
the details of the system studied). To take into account more easily
the 2-dimensional diffusion in the bottle (assumed to be a cylinder
of 56 mm diameter and 160 mm height), the mathematical model
was implemented in COMSOL3.5Ò (COMSOL Multiphysics) and then
exported into MatlabÒ software (The Mathworks Inc., Natick, MA)
to draw the figures.
In a first instance, the cap of the bottle was assumed to be
impermeable and only the OTR of the PET bottle was considered.
As shown in Fig. 5A for standard PET bottles, the model used with
this assumption predicted quite well the experimental results of
ascorbic acid losses (RMSE1 of 34.2 mg l1, less than 10% of error
on the predicted ascorbic losses; Fig. 5A) whereas fitting of the local
O2 content in the juice is obviously not as good (more than 30% of
error at 180 days; Fig. 5B). The high discrepancy between theoretical
and experimental results for O2 suggests an additional flux of O2
would occur in the bottle that could come from the closure. Experi-
1
Root Mean Square Error between the experimental data and the predicted one.
mental determination of the permeability of the cap being unfeasi-
ble, an identification of this parameter was attempted on the basis
of O2 experimental results. With an average thickness value of
1 mm, a permeability of 3  1017 mol m1 s1 Pa1 was found opti-
mal to fit the O2 data (Fig. 6B – dotted line, RMSE lower than 10%).
This value is in agreement with literature data about permeability
of HPDE (2.49 and 4.98  1017 mol m1 s1 Pa1 (Monsivais-Bar-
ron, Bonilla-Rios, Ramos de Valle, & Palacios, 2013). However, in that
case, the fitting of the ascorbic acid losses was less good; the RMSE
increased from 34.2 to 44.6 mg l1. Discrepancies between experi-
mental and predicted ascorbic losses could be explained by the ex-
tremely simplified oxidation mechanism represented by Eq. (1).
Obviously impact of O2 on ascorbic acid losses was not completely
well represented by Eq. (1); i.e. less O2 was required in practise than
in theory to oxidise ascorbic acid in the standard PET bottle. The stoi-
chiometry of the reaction used by Pénicaud et al. (2011) in their
work carried out in aqueous solutions may not completely fulfil
the conditions encountered in orange juice. In addition, the oxidative
pathway may not be the unique and predominant mode of degrada-
tion for ascorbic acid in orange juice (i.e. non-oxidative pathway,
Maillard reactions, hydrolysis) and, in that case, it is understandable
 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836 3835

Position of the
O2sensor

500

Local oxygen content (mg/L)

0.8
400
Ascorbic acid (mg/L)

0.6
300

0.4
200

100 0.2

0 0
0 50 100 150 0 5 10 15
Time (s) 6
Time (d) x 10

A B

500

0.8
Local O2 content (mg/L)

400
Ascorbic acid (mg/L)

0.6
300

0.4
200

0.2
100

0 0
0 50 100 150 0 5 10 15
6
Time (d) Time (s) x 10
C D
Fig. 5. Experimental (symbols) and predicted (solid and dotted lines) average ascorbic acid concentration and local content of dissolved O2 in orange juice stored at 20 °C and
400 lux in standard PET (A and B) and in active PETOS1 (C and D) bottles of 250 ml. Solid lines were obtained assuming that the cap was impermeable and dotted lines for a
permeable cap with an adjusted oxygen permeability. Experimental measurement and prediction of O2 content was for a position of 2 cm below the neck and against the
interface of the bottle.

that Eq. (1) was not able to correctly represent degradation of ascor-
bic acid.
In order to confirm the aforementioned hypothesis, the predic-
tions of the model were applied to a second set of data, those ob-
tained for the active PET (PETOS1). As shown in Fig. 5C and D, for
active PET, using the permeability of the cap previously identified,
predictions of local oxygen content were quite good (RMSE of 12%)
whereas prediction of ascorbic acid losses was worse than for stan-
dard PET (RMSE of 60.0 mg l1). Indeed, experimental points varied
on both sides of the theoretical curve: in practise, ascorbic acid
would degrade more rapidly than in theory during the first 15 days
of storage, then this degradation slowed down and became overes-
timated by the model. This confirms that the role of O2 in ascorbic
acid degradation in orange juice would be not as constant as pre-
dicted by Eq. (1) otherwise this experimental curve would have
been linear most of the time like the theoretical one. Further work
should be addressed in the future to clarify the modelling of ascor-
bic acid degradation in a real product when different mechanisms
coexist. This mathematical model, even if imperfect in its predic-
tions, pointed out the role of the closure in the O2 ingress into
the packaging. Due to this phenomenon, and also the monitoring
of local concentration (close to the interface of juice/headspace),
local O2 content was not so different between the two kinds of
PET in spite of differences in O2 average content and consequent
ascorbic acid losses. Without mathematical modelling, this unex-
pected behaviour of the O2 curve would not have been explained.
It is also important to note that uncertainty on the exact position
of the dot used to monitor local O2 made the analysis of O2 data dif-
ficult and revealed a limit of such non-invasive and non-destruc-
tive methods.
4. Conclusion
This study has confirmed that the ascorbic acid losses are the
most relevant marker of orange juice ageing and quality evolution
during storage. O2 was obviously the limiting parameter in the
reaction of ascorbic acid degradation and was consumed gradually
as it entered the package depending on its O2 permeability proper-
ties. Contrary to ascorbic acid, the aroma changes as a function of
time were not relevant markers of oxygen ingress and permeability
properties of the packaging. Indeed, the modification of the aroma
3836 C. Bacigalupi et al. / Food Chemistry 141 (2013) 3827–3836
profile seems mainly due to acid-catalysed reactions and to a lesser
extent to oxidation. After 6 months of storage, the losses of aroma
compounds can be drastic since they reached 30–100% of the initial
level, depending on the light intensity and nature of the com-
pounds. Exposure to extreme light condition (=10,000 lux) was
found to speed up ascorbic acid and aroma compound degradation,
inducing the formation of oxidative derivatives. A first attempt of
shelf life prediction was made using a mechanistic model coupling
O2 diffusion and the reaction of ascorbic acid degradation. Simula-
tions confirmed that permeation through packaging material and
especially through the closure need to be considered and that
mechanisms of ascorbic acid degradation must be better character-
ised, in order to propose more accurate predictions. At the mo-
ment, this model is able to predict the shelf life of orange juice
with less than 20% error and, used in a reverse manner, is able to
identify the window of O2 permeability required for maintaining
a minimal level of ascorbic acid (chosen by the user).
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