Effect of packaging and storage conditions on quality of shelled walnuts

S.F. Mexis
a
, A.V. Badeka
a
, K.A. Riganakos
a
, K.X. Karakostas
b
, M.G. Kontominas
a,
*
a
Laboratory of Food Chemistry and Technology, Department of Chemistry, University of Ioannina, Ioannina 45110, Greece
b
Section of Statistics, Department of Mathematics, University of Ioannina, Ioannina 45110, Greece
a r t i c l e i n f o
Article history:
Received 3 July 2008
Received in revised form 16 September
2008
Accepted 24 September 2008
Keywords:
Walnuts
Packaging
Shelf life
Quality
a b s t r a c t
The present study investigated the effect of packaging and storage conditions on quality of raw shelled
walnuts. Walnut kernels were packaged in: (a) low density polyethylene (LDPE), 55 lm in thickness in
air, (b) polyethylene terephthalate||polyethylene (PET||PE), 70 lm in thickness under N
2
, and (c) PET-
SiO
x
||PE pouches, 62 lm in thickness under N
2
. Samples were stored either under uorescent light or
in the dark at 4 or 20 C for a period of 12 months. Quality parameters monitored were peroxide value
(PV), hexanal, 2-thiobarbituric acid (TBA), odor, and taste of product. PV ranged between 0.3 for fresh
walnut kernels and 31.4 meq O
2
/kg oil for walnuts packaged in PE pouches exposed to light after 12
months of storage. Respective values for hexanal were <28.5 lg/kg and 36.0 mg/kg and for TBA ca. 0.2
and 11 mg MDA/kg. Values for odor ranged between 0.2 for fresh walnut kernels and 5.7 for walnut ker-
nels packaged in PE exposed to light after 12 months of storage at 20 C. Respective values for taste were
0.7 and 6.8. Taste proved to be a more sensitive attribute than odor. Based on shelf life (taste) values and
PV data it is proposed that the upper limit value for PV is close to 10.0 meq O
2
/kg walnut oil. Respective
limit values for hexanal are 12 mg hexanal/kg walnut and for TBA is 12 mg malondialdehyde/kg wal-
nut. Walnuts retained acceptable quality for ca. 2 months in PE-air, 45 months in PET||PE-N
2
and at least
12 months in PET-SiO
x
||PE-N
2
pouches at 20 C, with samples stored in the dark retaining slightly higher
quality than those exposed to light. The effect of parameters investigated followed the sequence: temper-
ature > degree of O
2
barrier > lighting conditions.
2008 Elsevier Ltd. All rights reserved.
1. Introduction
Walnuts are the edible fruit of any one of approximately 15 spe-
cies of walnut trees belonging to the Juglandaceae family. The wal-
nut is a highly appreciated nut because of its unique organoleptic
characteristics (Lopez, Pique, Romero, & Aleta, 1995), high levels
of 18:1, 18:2, and 18:3 fatty acids (Crews et al., 2005; Zwarts, Sa-
vage, & McNeil, 1999) and hypocholesterolemic (Abbey, Noakes,
Belling, & Nestel, 1994; Sabat & Fraser, 1994), and antihyperten-
sive effects (Sabat & Fraser, 1994). Walnuts are utilized as shelled
whole kernels or ground kernels being used as ingredients of many
foodstuffs such as bakery products and confectionery as well as a-
voring agents in beverages and ice-cream.
Walnut kernels have a lipid content of 65% (Vanhanen & Savage,
2006) of which 73% consists of polyunsaturated fatty acids (PUFA)
(Crews et al., 2005), although values do vary between cultivars
(Zwarts et al., 1999). These highlevels of PUFAs make walnuts prone
to oxidation. Besides the nature of PUFA, many other factors inu-
ence the oxidation potential of walnuts. These include: oxygen con-
centration (Jensen, Sorensen, Brockhoff, & Bertelsen, 2003; Jensen,
Sorensen, Engelsen, &Bertwlsen, 2001;Pastorelli et al., 2007; Pastor-
elli, Valzacchl, Rodriguez, & Simoneau, 2006), temperature (Jensen
et al., 2001; Jensen et al., 2003; Pastorelli et al., 2007), relative
humidity (Mat, Saltveit, & Krochta, 1996; Reed, Sims, Gorbet, &
OKeefe, 2002), light (Dominguez, Azuara, Vernon-Carter, & Beri-
stain, 2007; Jensen et al., 2001), antioxidants (Talcott, Duncan,
Pozo-Insfran, & Gorbet, 2005; Zacheo, Cappello, Gallo, Santino, &
Cappello, 2000), and method of processing (Adebiyi, Adeyemi, &
Jlorunda, 2002; Garcia-Pascual, Mateos, Carbonell, &Salazar, 2003).
Oxygen concentration is one of the most important extrinsic
factors affecting lipid oxidation. The rate of oxidation is indepen-
dent of oxygen concentration at very high oxygen partial pressures,
while it is proportional to oxygen concentration at low oxygen
partial pressures (Labuza, 1971). The availability of oxygen in a
package can, to a certain extent, be controlled by the oxygen per-
meability of the packaging material (Jensen et al., 2003). Jensen
et al. (2001) investigated the effect of storage conditions on walnut
quality using transparent and aluminum coated plastic laminates
to compare storage under light and in the dark. To accelerate lipid
oxidation they ushed the packages with approximately 50% O
2
and 50% N
2
during packing before storage at two temperatures (5
and 21 C). The study established that storage under light results
in pronounced oxidative changes in walnuts especially at 21 C,
where as storage in the dark at 5 C results in walnuts without
any trace of rancid taste after 25 weeks of storage even under
0956-7135/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.foodcont.2008.09.022
* Corresponding author. Tel.: +30 26510 98342.
E-mail address: mkontomi@cc.uoi.gr (M.G. Kontominas).
Food Control 20 (2009) 743751
Contents lists available at ScienceDirect
Food Control
j our nal homepage: www. el sevi er . com/ l ocat e/ f oodcont
accelerated conditions (50% oxygen). In another study, Jensen et al.
(2003) studied the oxidation of walnuts packed in three different
packaging materials namely: low density polyethylene (LDPE),
polyethylene terephthalate||polyethylene (PET||PE), and polyethyl-
ene/ethylene-vinyl alcohol/polyethylene (PE/EVOH/PE) and stored
in the dark at either 11 or 21 C. The walnuts were packed under
air in LDPE and either under air, N
2
or O
2
absorbers for PET||PE
and PE/EVOH/PE. They found that the optimal storage temperature
for walnuts was 11 C or lower, preferably combined with use of an
O
2
absorber. However, without chilled storage and use of an oxy-
gen absorber, it was possible to obtain walnuts of acceptable qual-
ity with a high barrier packaging material combined with N
2
ushing for 13 months.
Storage temperature can have a dramatic effect on oxidation
rate, which in turn affects off-avor formation. Several studies
have focused on the inuence of storage conditions on pistachio,
almond, peanut, and walnut at high temperatures such as 30, 36,
and 40 C. Results showed nuts to be dramatically more rancid as
compared to those stored at 8, 10, 20 or 25 C for the same period
of time (Braddock, Sims, & OKeefe, 1995; Crowe & White, 2003;
Garcia-Pascual et al., 2003; Maskan & Karatas, 1999; Nepote, Mes-
trallet, Accietto, Galizzi, & Grosso, 2006).
The objective of the present study was to investigate the effect
of (1) packaging material barrier to light and oxygen, (2) head
space composition, and (3) storage temperature on quality reten-
tion of whole walnut kernels.
2. Material and methods
2.1. Materials
Walnut kernels were supplied by Sdoukos SA Ioannina, Greece
in November 2006 packed in berboard cartons with an inner PE
lm, 10 kg per carton. They had been harvested during the period
SeptemberOctober 2006, mechanically shelled and packaged as
described above. Experiments were carried out during the period
November 2006November 2007.
2.2. Experimental design
Walnut kernels were packaged in three different packaging
materials: (a) LDPE, 55 lm in thickness and 4500 mL/(m
2
day atm)
in oxygen permeability in air, (b) PET||PE, 70 lm in thickness and
103 mL/(m
2
day atm) in oxygen permeability, and (c) PET-SiO
x
||PE,
62 lm in thickness and 1.4 mL/(m
2
day atm) in oxygen permeabil-
ity measured using the Oxtran 2-20 oxygen permeability tester
(MOCON Co. Minneapolis, MN, USA), at 0% RH and 22 C. Pouches
(PET||LDPE and PET-SiO
x
||LDPE) containing walnuts (100 g) were
rst evacuated and then immediately injected the N
2
produced by
a PBI Dansensor MAP Mix 9000 gas mixer (Dansensor, Ringsted,
Denmark). Pouches were heat-sealedusing a BOSS model NE 48 vac-
uumsealer (BOSS, Bad Homburg, Germany) and stored either under
uorescent light (825 50 lux) or in the dark at either 4 or 20 C.
Reference samples were prepared by packaging walnut kernels in
glass jars ushed with N
2
and stored at 18 C for up to 12 months.
After 0, 2, 4, 6, 8, 10, and 12 months of storage, three separate iden-
tical samples were withdrawn from each treatment for chemical
and sensory analysis. Duplicate measurements were carried out
on each of three replicate samples for chemical analysis (n = 6).
2.3. Methods
2.3.1. Gas composition
At each sampling day, the headspace gas composition in each
pouch was determined using a Dansensor CheckMate 9900
gaspace analyzer (PBI, Ringsted, Denmark). Gas analysis was per-
formed by drawing a headspace gas sample by piercing a syringe
needle through a rubber septum glued on the surface of the PET||PE
and PET-SiO
x
||PE pouches.
2.3.2. Extraction of fat-peroxide value
The oil of walnuts was extracted using the Welmann method:
crushed walnuts (5 g) were transferred into a separatory funnel
with 100 mL of diethyl ether and 10 mL of distilled water. The
separatory funnel was agitated for a few minutes and subsequently
left to equilibrate for 24 h. 50 mL of the sample were transferred in
a crystallizing dish and diethyl ether evaporated in a water bath at
40 C. The extracted oil was dried in an oven at 105 C for 3 min,
and the residue was used for determination of the peroxide value.
The peroxide value was determined according to the ofcial EC
(2568/91) method for the measurement of the characteristics of ol-
ive oil and olive-residue oil.
2.3.3. 2-Thiobarbituric acid (TBA)
TBA was determined according to the method of Gomes, Silva,
Nascimento, and Fukuma (2003) as modied by Goulas and Kon-
tominas (2007). The method is based on the spectrophotometric
quantitation of the pink complex formed after reaction of one mol-
ecule of malondialdehyde (MDA), product of distillation, with two
molecules of 2-thiobarbituric acid (TBA) added to the distillate.
2.3.4. HexanalSPME procedure
Walnut samples (0.1 g), along with 1 mL of distilled water and a
micro-stirring bar were placed in a 10 mL glass serum vial which
was sealed with an aluminum crimp cap provided with a needle-
pierceable polytetrauroethylene/silicone septum. Solid-phase
microextraction (SPME) was performed with a 75-lm carboxen/
polydimethylsiloxane (PDMS) bre mounted to a SPME manual
holder assembly (Supelco, Bellefonte, USA) as previously described
(Karatapanis, Badeka, Riganakos, Savvaidis, & Kontominas, 2006).
Hexanal was identied using a hexanal standard (Fluka Chemie
GmbH, Buchs, Switzerland) and quantied using a calibration
curve.
2.3.5. GCFID analysis conditions
GC analysis of hexanal adsorbed onto the SPME bre was car-
ried out on a HewlettPackard HP 5890 series II GC unit (Wilming-
ton, USA) equipped with a FID. A capillary column HP-5 (J&W
Scientic, Folsom, USA) 30 m long, 0.32 mm in internal diameter
and 0.25 lm in thickness was used. The GC oven was programmed
as follows: the temperature was initially set at 40 C for 5 min, and
then raised at the rate of 15 C/min to 230 C. The injector temper-
ature was set to 270 C in split mode (2:1 split ratio) and detector
temperature was kept at 330 C. Flow rate of the helium carrier gas
was 0.8 mL/min. For thermal desorption, the SMPE bre was kept
in the injector for 10 min. Data was performed using HP GC Chem-
station software for Windows (HewlettPackard).
2.3.6. Sensory evaluation
The samples for sensory evaluation (consumer analysis) were
evaluated by a 51 member panel. Panelists were chosen using the
following criteria: ages between 18 and 60, non-smokers, without
reported cases of food allergies who consumed dried nut products
regularly. For sample evaluation the panelists were served a control
reference sample (stored at 18 C) along with the test samples.
Approximately 20 g of walnuts were placed in small plastic cups
coded with 3-digit random numbers and tightly capped. The sam-
ples were allowed to stand for 30 min prior to the evaluation, to al-
low equilibration of volatiles in the headspace. The samples were
presented to panelists in random order at 20 C with water and pa-
per ballots ona tray. Panelists were instructedtoconsume the whole
744 S.F. Mexis et al. / Food Control 20 (2009) 743751
sample and rinse mouth with sparkling water (room temperature),
in between sample evaluation. A ten point hedonic scale ranging
from 0 to 9, where 0 = extremely like and 9 = extremely dislike
was usedto evaluate acceptability of sample (odor, taste). The upper
limit of acceptability corresponded to a score of 4, while develop-
ment of a slightly rancid (taste/odor) corresponded to a score of 3.
2.4. Statistical analysis
Data were subjected to analysis of variance (ANOVA) using the
software SPSS 16 for Windows. Means and standard deviations
were calculated, and, when F-values were signicant at the
p < 0.05 level, mean differences were separated by the least signif-
icant difference procedure.
3. Results and discussion
3.1. Gas composition
N
2
concentrations for PET||PE and PET-SiO
x
||PE as a function
of lighting conditions, temperature, and storage time are given in
Table 1. Data in Table 1 shows that for PET||PE packaged walnuts,
after 2 months the N
2
concentration fell below 98% exposing the
product to O
2
. In contrast, the high barrier material PET-SiO
x
||PE
even after 12 months of storage retained a N
2
concentration above
or equal to 99.8% effectively protecting the product from oxidation.
3.2. Lipid oxidation
3.2.1. Peroxide value
Lipid oxidation of walnuts was evaluated by measuring perox-
ide value (PV), hexanal (an oxidation product of linoleic acid) and
malondialdehyde (an oxidation product of linolenic acid). Changes
in PV are shown in Fig. 1a and b. The initial PV of fresh walnuts was
very low (0.3 meq O
2
/kg walnut oil). Fig. 1a shows the effect of
storage time, packaging material, and light on PV at 20 C. Both
storage time and packaging material signicantly (p < 0.05) af-
fected peroxide value. After 12 months of storage walnuts pack-
aged in the PET-SiO
x
||PE pouches had a very low PV ca. 3
3.3 meq O
2
/kg walnut oil irrespective on lighting conditions.
Respective PV was 12.6 meq O
2
/kg walnut oil for walnuts packaged
in PET||PE in the dark, 20.0 meq O
2
/kg walnut oil packaged in
PET||PE exposed to light and PE stored in the dark and nally ca.
31.4 meq O
2
/kg walnut oil packaged in PE exposed in light. Like-
wise, Fig. 1b shows the respective effect of packaging material O
2
barrier and light on PV at 4 C. After 12 months of storage walnuts
packaged in the PET-SiO
x
||PE pouches had a PV ca. 2.8 meq O
2
/kg
walnut oil irrespective of lighting conditions. Respective PV was
ca. 10.0 O
2
/kg walnut oil packaged in PET||PE stored in the dark,
14.0 meq O
2
/kg walnut oil packaged in PET||PE exposed to light,
11.8 meq O
2
/kg walnut oil packaged in PE in the dark and nally
15.0 meq O
2
/kg walnut oil packaged in PE exposed to light. A sec-
ond observation is that for a given temperature, exposure to light
resulted in higher PVs as compared to storage in the dark with
the exception of the high barrier material PET-SiO
x
||PE. Compari-
son of data in Fig. 1a and b leads to the conclusion that as the O
2
barrier of the packaging material decreased, the effect of tempera-
ture was more signicant. Also for products packed in LDPE, stor-
age temperature had a more pronounced effect than light. For
products packaged in PET||PE the effect of temperature was similar
to that of light. Finally for products packaged in PET-SiO
x
||PE the ef-
fect of both temperature and light was negligible.
According to Savage, McNeil, and Osterberg (2001) fresh wal-
nuts had a PV ranging from 0.05 to 0.29 meq O
2
/kg walnut oil. Jen-
sen et al. (2001) packaged walnut kernels in high barrier
transparent and aluminum coated plastic laminates and reported
PV ca. 3.5 meq O
2
/kg walnut oil for products stored in the dark at
5 C, 4.9 meq O
2
/kg walnut oil for products stored in the dark at
21 C and 8.0 meq O
2
/kg walnut oil for walnuts stored at 21 C irre-
spective of lighting conditions after 25 weeks of storage. These val-
ues are higher than those of the present work in the range of
2.0 meq O
2
/kg walnut oil. Differences may be attributed to the
accelerated conditions of storage (50% O
2
) used in the former work.
Mat et al. (1996) studied the inuence of O
2
concentration and
relative humidity on the rancidity of walnuts and reported PV be-
tween 1 and 2 meq O
2
/kg walnut oil for products stored at low O
2
(<2.5%) and either 21% or 53% RH at 37 C. Respective PV for high
O
2
(21%) storage after 10 months were 5.0 meq O
2
/kg walnut oil
at 21% and 13.5 meq O
2
/kg walnut oil at 53% RH. Peroxide values
of walnuts packaged in low O
2
environments are similar to those
reported in the present study given the differences in experimental
temperatures employed.
3.2.2. Hexanal content
Changes in hexanal are shown in Fig. 2a and b. The initial hex-
anal content of fresh walnuts was lower than the method detection
limit (28.5 lg/kg). Fig. 2a shows the effect of storage time, packag-
ing material, and light on hexanal content at 20 C. After 12 months
of storage, walnuts packaged in PET-SiO
x
||PE pouches had very low
ca. 2.0 mg hexanal/kg walnut irrespective of lighting conditions.
Respective hexanal values were ca. 12.0 mg hexanal/kg walnuts
packaged in PET||PE stored in dark, 28 mg hexanal/kg for walnuts
packaged in PET||PE exposed in light, 27 mg hexanal/kg walnuts
packaged in PE stored in the dark, and nally 36.0 mg hexanal/kg
for walnuts packaged in PE exposed to light. Likewise Fig. 2b shows
the respective effect of packaging material O
2
barrier and light on
hexanal content at 4 C. After 12 months of storage walnuts pack-
aged in the PET-SiO
x
||PE pouches had a hexanal content of ca.
Table 1
Changes in headspace N
2
of stored walnuts under various packaging conditions.
0 Month 2 Month 4 Month 6 Month 8 Month 10 Month 12 Month
N
2
(%) SD N
2
(%) SD N
2
(%) SD N
2
(%) SD N
2
(%) SD N
2
(%) SD N
2
(%) SD
Light 20 C PET||LDPE 99.9
g
0.1 96.3
f
0.2 89.9
e
0.5 88.0
d
0.3 87.1
c
0.1 85.1
b
1.3 83.0
a
0.2
Light 4 C PET||LDPE 99.9
f
0.1 97.7
e
0.1 90.5
d
0.4 88.5
c
0.4 87.1
b
0.6 86.4
b
0.2 84.1
a
0.4
Dark 20 C PET||LDPE 99.9
e
0.1 91.1
d
0.3 87.0
c
0.3 87.3
c
0.1 86.0
b
0.5 84.0
a
0.1 83.7
a
0.7
Dark 4 C PET||LDPE 99.9
e
0.1 95.0
d
0.7 88.6
c
0.5 88.6
c
0.5 86.6
b
0.3 86.3
b
0.5 84.2
a
0.5
Light 20 C PET-SiJ
x
||LDPE 99.9
a
0.1 99.9
a
0.1 99.9
a
0.1 99.9
a
0.0 99.9
a
0.0 99.9
a
0.0 99.8
a
0.1
Light 4 C PET-SiJ
x
||LDPE 99.9
a
0.1 99.9
a
0.0 99.9
a
0.0 99.9
a
0.1 99.9
a
0.1 99.9
a
0.2 99.8
a
0.2
Dark 20 C PET-SiJ
x
||LDPE 99.9
a
0.1 99.8
a
0.2 99.9
a
0.2 99.9
a
0.1 99.9
a
0.1 99.9
a
0.1 99.8
a
0.1
Dark 4 C PET-SiJ
x
||LDPE 99.9
a
0.1 99.9
a
0.0 99.9
a
0.1 99.9
a
0.0 99.9
a
0.0 99.9
a
0.0 99.8
a
0.7
Mean value (n = 6), SD.
ag
Means with different superscripts are statistically different (p < 0.05).
S.F. Mexis et al. / Food Control 20 (2009) 743751 745
0.2 mg hexanal/kg walnuts irrespective of lighting conditions.
Respective hexanal content was 4.4 mg hexanal/kg walnuts pack-
aged in PET||PE in the dark, 5.8 mg hexanal/kg for walnuts pack-
aged in PET||PE exposed to light, 8.7 mg hexanal/kg for walnuts
packaged in PE in the dark, and nally 9.4 mg hexanal/kg for wal-
nuts packaged in PE exposed to light.
A second observation is that for a given temperature exposure
to light resulted in higher hexanal concentrations as compared to
storage in the dark with the exception of the high barrier material
PET-SiO
x
||PE.
Comparison of data in Fig. 2a and b leads to the conclusion that
as the packaging materials O
2
barrier decreased, the effect of tem-
perature increased. Also for products packaged in PE and PET||PE
the effect of storage temperature was more pronounced than the
effect of light. For products packaged in PET-SiO
x
||PE the effect of
both temperature and light were negligible. Jensen et al. (2001)
packaged walnut kernels in high barrier transparent and alumi-
num coated plastic laminates and reported hexanal values of ca.
5.0 mg hexanal/kg for products stored in the dark at 5 C,
25.0 mg hexanal/kg for products packaged under light at 5 C,
70.0 mg/kg for products stored under dark at 21 C, and nally
185.0 mg/kg for products stored under light at 21 C. These values
are higher than those of the present work in the range of 0.51 mg/
kg. Differences may be attributed to the high concentration of O
2
(50%) used in the former study to achieve accelerated storage con-
ditions. In a similar study, Jensen et al. (2003) stored walnut ker-
nels in three different packaging material (PE, PET||PE, oriented
polyamide (OPA)/EVOH/PE) in the dark at 11 and 21 C using either
air, N
2
or O
2
absorbers for 13 months and reported hexanal values
ca. 210 mg/kg for walnuts packaged in PET||PE at 21 C and <5 mg/
kg for walnuts packaged in OPA/EVOH/PE at 21 C under a N
2
atmosphere. Values for products packaged in the high barrier
material are in excellent agreement with values recorded for
PET-SiO
x
||PE at 20 C in the present study. However, hexanal values
for products packaged in PET||PE are much higher than those re-
ported in the present study (210.0 vs. 12.0 mg/kg). Such large dif-
Fig. 1. Changes in peroxide value of walnuts as a function of packaging material oxygen barrier, lighting conditions, and storage time at (a) 20 C and (b) 4 C.
746 S.F. Mexis et al. / Food Control 20 (2009) 743751
ferences may be due to pinholes in the packaging material used, as
the above authors speculate.
Mat et al. (1996) studied walnut rancidity as inuenced by O
2
concentration and relative humidity and reported a hexanal con-
tent less than 10.0 mmol/g 10
6
(1 mg/kg) for products stored
at low O
2
(<2.5%) and either 21% and 53% RH. Respective hexanal
content for high O
2
storage was ca. 30.0 mmol/g 10
6
(3.0 mg/
kg) at 21% RH, and 430.0 mmol/g 10
6
(43.0 mg/kg) at 53%
RH. Hexanal content of walnuts packaged in the low O
2
environ-
ment are in good agreement with those reported in the present
study given the differences in experimental temperatures
employed.
3.2.3. Thiobarbituric acid
Changes in malondialdehyde values are shown in Fig. 3a and b.
Fig. 3a shows the effect of storage time, packaging material, and
light on malondialdehyde content at 20 C. As with hexanal, stor-
age time and packaging material signicantly (p < 0.05) affected
malondialdehyde content. After 12 months of storage, walnuts
packaged in PET-SiO
x
||PE pouches had a very low, ca. 2.0 mg
MDA/kg irrespective of lighting conditions. Respective malondial-
dehyde content was ca. 7.7 mg/kg for walnuts packaged in PET||PE
stored in dark, 9.7 mg/kg for walnuts packaged in PET||PE exposed
to light, 9.8 mg/kg for walnuts packaged in PE stored in the dark,
and nally 11.0 mg/kg for walnuts packaged in PE exposed to light.
Likewise, Fig. 3b shows the respective effect of packaging material
O
2
barrier and light on malondialdehyde content at 4 C. After 12
months of storage malondialdehyde content was ca. 1.2 mg/kg
for walnuts packaged in PET-SiO
x
||PE stored in the dark, 2.2 mg/
kg for walnuts packaged in PET-SiO
x
||PE exposed to light, 2.6 mg/
kg for walnuts packaged in PE stored in the dark, 3.1 mg/kg for
walnuts packaged in PET||PE stored in the dark, 4 mg/kg for wal-
nuts packaged in PET||PE exposed to light, and nally 5.1 mg/kg
for walnuts packaged in PE exposed to light.
Fig. 2. Changes in hexanal content of walnuts as a function of packaging material oxygen barrier, lighting conditions, and storage time at (a) 20 C and (b) 4 C.
S.F. Mexis et al. / Food Control 20 (2009) 743751 747
For a given temperature, exposure to light resulted in a higher
(p < 0.05) malondialdehyde content compared to storage in the
dark. As with hexanal, the highest malondialdehyde values were
recorded for products packaged in PE exposed to light at 20 C
and the lowest malondialdehyde values, for products packaged in
PET-SiO
x
||PE stored in the dark at 4 C. Comparison of data in
Fig. 3a and b leads to the conclusion that as the packaging mate-
rials O
2
barrier decreased the effect of temperature increased. Also
for all packaging treatments the effect of temperature was more
pronounced than that of light.
3.3. Sensory evaluation
Results of assessment of odor and taste of walnuts are shown
in Figs. 4a and b and 5a and b. As shown in Fig. 4a, after 12
months of storage at 20 C, odor changes were the least in
products packaged in PET-SiO
x
||PE (score 1.82.0) irrespective of
lighting conditions while the most pronounced changes in odor
were recorded in products packaged in PE exposed to light (score
5.7). Respective scores at 4 C were 1.71.8 for PET-SiO
x
||PE irre-
spective of lighting conditions and 5.3 for PE exposed to light.
Products packaged in PET||PE received intermediate scores at both
temperatures.
As shown in Fig. 5a, after 12 months of storage at 20 C taste
changes were the least in PET-SiO
x
||PE (score 3.43.6) irrespective
of lighting conditions while most pronounced changes in taste
were recorded in products packaged in PE exposed to light (score
6.8). Respective scores at 4 C were 3.73.8 for PET-SiO
x
||PE irre-
spective of lighting conditions and 6.3 for PE exposed to light. Taste
proved to be a more sensitive sensory attribute for quality assess-
ment of walnuts than odor. Based on taste and an upper accept-
ability limit of 4 it can be stated that the shelf life of fresh
walnuts at 20 C is less than or equal to 2 months packaged in PE
pouches in air, 45 months packaged in PET||PE pouches in N
2
and at least 12 months packaged in PET-SiO
x
||PE pouches in N
2
.
At 4 C shelf life is 4 months in PE pouches exposed to light, 5.5
Fig. 3. Changes in malondialdehyde content of walnuts as a function of packaging material oxygen barrier, lighting conditions, and storage time at (a) 20 C and (b) 4 C.
748 S.F. Mexis et al. / Food Control 20 (2009) 743751
months in PE pouches stored in the dark, 5 months in PET||PE ex-
posed to light, 8 months in PET||PE stored in the dark, and at least
12 months in PET-SiO
x
||PE irrespective of lighting conditions.
Based on shelf life (taste) values and data in Fig. 1a and b it is pro-
posed that the upper limit value for PV is close to 10.0 meq O
2
/kg
walnut oil. Respective limit values for hexanal are 12 mg hexanal/
kg walnut and for TBA is 12 mg malondialdehyde/kg walnut. To
the best of our knowledge this is the rst time such limits have
been proposed.
Jensen et al. (2003) stored walnut kernels in different packaging
materials (PE, PET||PE, and OPA/EVOH/PE) in the dark at 11 and
21 C using either air, N
2
or O
2
absorbers for 13 months. They re-
ported that PE-air, PET||PE-air and PET||PE-N
2
were rated as very
rancid after 5 months of storage while walnuts packaged in OPA/
EVOH/PE-N
2
became slightly rancid after 7 months of storage.
However, walnuts packaged along with O
2
absorbers and stored
at 11 or 21 C maintained the same quality as the reference sample
(stored at 18 C in the dark). These sensory data are in good
agreement with data reported in the present study.
4. Conclusion
The present study investigated the effect of packaging material
O
2
barrier, lighting conditions, and temperature on quality of
shelled walnuts as a function of storage time. It was shown that
walnuts retain acceptable quality for ca. 2 months in PE-air, 45
months in PET||PE-N
2
and at least 12 months in PET-SiO
x
||PE-N
2
pouches at 20 C with samples stored in the dark retaining slightly
higher quality than those exposed to light. The effect of parameters
investigated follows the sequence: temperature > degree of O
2
bar-
rier > lighting conditions.
Fig. 4. Changes in odor of walnuts as a function of packaging material oxygen barrier, lighting conditions, and storage time at (a) 20 C and (b) 4 C.
S.F. Mexis et al. / Food Control 20 (2009) 743751 749
References
Abbey, M., Noakes, M., Belling, B. G., & Nestel, P. J. (1994). Partial replacement of
saturated fatty acids with almonds or walnuts lowers total plasma cholesterol
and low-density-lipoprotein cholesterol. American Journal of Clinical Nutrition,
59, 995999.
Adebiyi, A. P., Adeyemi, I. A., & Jlorunda, A. O. (2002). Effects of processing
conditions and packaging material on the quality attributes of dry-roasted
peanuts. Journal of the Science of Food and Agriculture, 82, 14651471.
Braddock, J. C., Sims, F. C., & OKeefe, S. F. (1995). Flavor and oxidative stability of
roasted high oleic acid peanuts. Journal of Food Science, 60(3), 489493.
Commission Regulation (EC) (1991). No. 2568/91 of 11 July 1991 on the
characteristics of olive oil and olive-residue oil and on the relevant methods
of analysis. Ofcial Journal of the European Communities, L 248, 182.
Crews, C., Hough, P., Godward, J., Brereton, P., Lees, M., Guiet, S., et al. (2005). Study
of the main constituents of some authentic walnut oils. Journal of Agricultural
and Food Chemistry, 53, 48534860.
Crowe, T. D., & White, P. J. (2003). Oxidation, avour and texture of walnuts reduced
in fat content by supercritical carbon dioxide. Journal of the American Oil
Chemists Society, 80(6), 569574.
Dominguez, I. L., Azuara, E., Vernon-Carter, E. J., & Beristain, C. I. (2007).
Thermodynamic analysis of the water activity on the stability of macadamia
nut. Journal of Food Engineering, 81, 566571.
Garcia-Pascual, P., Mateos, M., Carbonell, V., & Salazar, D. M. (2003). Inuence of
storage conditions on the quality of shelled and roasted almonds. Biosystems
Engineering, 87(2), 201209.
Gomes, H. A., Silva, E. N., Nascimento, M. R. L., & Fukuma, H. T. (2003). Evaluation of
the 2-thiobarbituric acid method for the measurement of lipid oxidation in
mechanically debonded gamma irradiated chicken meat. Food Chemistry, 80,
433437.
Goulas, A. E., & Kontominas, M. G. (2007). Combined effect of light salting, modied
atmosphere packaging and oregano essential oil on the shelf-life of sea bream
(Sparus aurata): Biochemical and sensory attributes. Food Chemistry, 100(1),
287296.
Jensen, P. N., Sorensen, G. B., Brockhoff, P., & Bertelsen, G. (2003). Investigation of
packaging systems for systems for shelled walnuts based on oxygen absorbers.
Journal of Agricultural and Food Chemistry, 51, 49414947.
Jensen, P. N., Sorensen, G., Engelsen, S. B., & Bertwlsen, G. (2001). Evaluation of
quality in walnut kernels (Junglans regia L.) by Vis/NIR spectroscopy. Journal of
Agricultural and Food Chemistry, 49, 57905796.
Karatapanis, E., Badeka, A., Riganakos, K., Savvaidis, I., & Kontominas, M. (2006).
Changes in avor volatiles of whole pasteurized milk as affected by
packaging materials and storage time. International Dairy Journal, 16, 750
761.
Labuza, P. (1971). Kinetics of lipid oxidation in foods. CRC Critical Reviews in Food
Technology, 2, 355405.
Fig. 5. Changes in taste of walnuts as a function of packaging material oxygen barrier, lighting conditions, and storage time at (a) 20 C and (b) 4 C.
750 S.F. Mexis et al. / Food Control 20 (2009) 743751
Lopez, A., Pique, M. T., Romero, A., & Aleta, N. (1995). Inuence of cold-storage
condition on the quality of unshelled walnuts. International Journal of
Refrigeration, 8, 544549.
Maskan, M., & Karatas, S. (1999). Storage stability of whole-split pistachio nuts
(Pistachia vera L.) at various conditions. Food Chemistry, 66, 227233.
Mat, J. I., Saltveit, M. E., & Krochta, J. M. (1996). Peanut and walnut rancidity:
Effects of oxygen concentration and relative humidity. Journal of Food Science,
61(2), 465469.
Nepote, V., Mestrallet, M. G., Accietto, R. H., Galizzi, M., & Grosso, N. R. (2006).
Chemical and sensory stability of roasted high-oleic peanuts from Argentina.
Journal of the Science of Food and Agriculture, 86, 944952.
Pastorelli, S., Torr, L., Rodriguez, A., Valzacchi, S., Limbo, S., & Simoneau, C. (2007).
Solid-phase micro-extraction (SPME-GC) and sensors as rapid methods for
monitoring lipid oxidation in nuts. Food Additives and Contaminants, 24(11),
12191225.
Pastorelli, S., Valzacchl, S., Rodriguez, A., & Simoneau, A. (2006). Solid-phase
microextraction method for the determination of hexanal in hazelnuts as an
indicator of the interaction of active packaging materials with food aroma
compounds. Food Additives and Contaminants, 23(11), 12361241.
Reed, K. A., Sims, C. A., Gorbet, D. W., & OKeefe, S. F. (2002). Storage water activity
affects avor fade in high and normal oleic peanuts. Food Research International,
35, 769774.
Sabat, J., & Fraser, E. (1994). Nuts: A new protective food against coronary heart
disease. Current Opinion in Lipidology, 5, 1116.
Savage, P., McNeil, L., & Osterberg, K. (2001). Oxidative stability of walnuts during
storage. 4th International walnut symposium. Acta Horticulturae, 544, 591597.
Talcott, S. T., Duncan, C. E., Pozo-Insfran, D. D., & Gorbet, D. W. (2005). Polyphenolic
and antioxidant changes during storage of normal, mid, and high oleic acid
peanuts. Food Chemistry, 89, 7784.
Vanhanen, L. P., & Savage, G. P. (2006). The use of peroxide value as a measure of
quality for our stored at ve different temperatures using three different types
of packaging. Food Chemistry, 99, 6469.
Zacheo, G., Cappello, M. S., Gallo, A., Santino, A., & Cappello, A. R. (2000). Changes
associated with post-harvest ageing in almonds seeds. Lebensmittel-
Wissenschaft und-Technologie, 33, 415423.
Zwarts, L., Savage, G. P., & McNeil, D. L. (1999). Fatty acid content of New Zealand-
grown walnuts (Juglans regia L.). International Journal of Food Sciences and
Nutrition, 50, 189194.
S.F. Mexis et al. / Food Control 20 (2009) 743751 751