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Polymeric-Based Food Packaging for High-Pressure Processing

Article  in  Food Engineering Reviews · December 2010

DOI: 10.1007/s12393-010-9026-0

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Food Eng. Rev. (2010) 2:274–297
DOI 10.1007/s12393-010-9026-0
Polymeric-Based Food Packaging for High-Pressure Processing
Pablo Juliano • Tatiana Koutchma •
Qian Sui • Gustavo V. Barbosa-Cánovas •
George Sadler
Received: 20 June 2010 / Accepted: 16 July 2010 / Published online: 10 August 2010
Ó Springer Science+Business Media, LLC 2010
Abstract High-pressure processing (HPP) of foods
mainly utilizes flexible packaging materials for commercial
products. Many materials have been evaluated for their
adequacy in the process. There are a number of integrity
requirements for these packaging materials that must be
complied with for acceptance and use in different product
applications. These include visual integrity, gas perme-
ability, seal and physical strength properties, and global
migration of packaging components into the food, some of
which are specific to either refrigerated or shelf-stable
products. Different laminate options reported in the liter-
ature were reviewed in this article with the aim of classi-
fying suitable packaging materials for HPP at both low-
and high-temperature conditions according to these
requirements. Packaging materials currently utilized in
industry are also listed. The suitability of standards to
assess requirement deviations after HPP is also discussed.
Current scientific literature has shown to lack information
P. Juliano (&)
CSIRO Food and Nutritional Sciences, 671 Sneydes Rd,
Werribee, VIC 3030, Australia
e-mail: Pablo.Juliano@csiro.au
T. Koutchma
Agriculture and Agri-Food Canada, Guelph, ON, Canada
Q. Sui
Department of Agricultural and Food Systems, Melbourne
School of Land and Environment, The University of Melbourne,
Parkville, VIC, Australia
G. V. Barbosa-Cánovas
Center for Nonthermal Processing of Food, Washington State
University, Pullman, WA, USA
G. Sadler
PROVE IT, LLC, West Lafayette, IN, USA
123
on one or more of these requirements to provide a complete
picture for their suitability. Studies have shown that
EVOH-based and other high-pressure–high-temperature-
treated materials do not follow the barrier requirements
established by the US Army for shelf-stable products.
However, they still show potential for their utilization in
the development of commercial products. The importance
of package headspace on package integrity is also high-
lighted. Studies on transport phenomena such as material
sorption and diffusion of components from the food and the
pressurization fluid are described. Methods such as SEM,
C-SAM, DSC, FT-IR, and X-Ray diffraction provide
complementary information to assess the structural and
barrier changes observed during HPP. The article con-
cludes by providing preliminary recommendations
according to specific requirements that are met after the
process. Other types of materials not yet evaluated for HPP
are presented as potential alternatives to be explored for
this technology.
Keywords Packaging  High-pressure processing 
Pouch  Sterilization  Pasteurization  Shelf stable 
Food
Abbreviations
Al Aluminum foil
AlOx Aluminum oxide
BOA Biaxially oriented polyamide
BON Biaxially oriented polyamide (‘‘nylon’’) film
BOPP Biaxially oriented polypropylene film
CFD Computational fluid dynamics
CPP Cast polypropylene
C-SAM Scanning acoustic microscopy
DSC Differential scanning calorimetry
EVA Ethylene–vinyl acetate
Food Eng Rev (2010) 2:274–297 275

EVOH Ethylene–vinyl alcohol industry. In batch HPP systems, the product is generally
FT-IR Fourier transform infrared treated in its final primary package; commonly, the food
HDPE High-density polyethylene and its packaging are treated together; thus, the entire
HPP High-pressure processing package remains a ‘‘secure unit’’ until the consumer opens
HP-HT High pressure–high temperature it. In-container processing requires packages in form of
HP-LT High pressure–low temperature pouches, large bulk bags, or container-lid combination.
KOP Polyvinylidene-coated BOPP film According to Lambert et al. [34], 90% of HPP-processed
LCP Liquid crystalline polymer foods are processed in flexible or partially rigid packages.
LDPE Low-density polyethylene Figure 1 shows examples of commercial polymeric bottles,
LLDPE Linear low-density polyethylene trays, and multilayer pouches currently utilized in industry.
MRE Meals-ready-to-eat High-pressure processing requires airtight packages that
METPET Metallized polyethylene terephthalate can withstand a change in volume corresponding to the
P Pressure (MPa) compressibility of the product. Foods decrease in volume
PA Polyamide (nylon) as function of the pressure applied and an equal expansion
PATS Pressure-assisted thermal sterilization occurs upon decompression. For this reason, the packaging
PATP Pressure-assisted thermal processing used for treated foods must be able to accommodate up to a
PE Polyethylene 19% reduction in volume and return to its original volume
PET Polyethylene terephthalate without loss of seal integrity or barrier properties. Pack-
PHBH Poly 3-hydroxy butyrate co 3-hydroxy aging materials, which are oxygen impermeable and opa-
hexanoate que to light, have been developed for keeping colors and
PP Polypropylene flavors fresh in certain HPP-treated foods. Some multilayer
PTFE Polytetrafluorethylene structures also may be suitable for pre-packaged high-
PVDC Poly(vinylidene chloride) pressure-treated foods. At least one interface in the package
PVOH Poly(vinyl alcohol) should be flexible enough to transmit the pressure. There-
SEM Scanning electron microscopy fore, rigid metal, glass, some plastic containers, or paper
SiOx Silicon oxide
T Temperature (K)
t Time (s)
USDA US Department of Agriculture
US FDA US Food and Drug Administration

Processing Foods with High Hydrostatic Pressure

High-pressure processing (HPP) of foods is an emerging

technology applied for safety assurance, shelf-life exten-
sion, and nutrient preservation. A number of commercial
products such as sliced meats, vegetables and salsa dips,
fruit juices, seafood products, and ready-to-eat chilled
products processed by applying HPP are available today in
the worldwide market [4, 53]. HPP is known for its
potential in manufacturing novel value-added foods
retaining heat-labile nutrients, flavors, and aromas, with
products ranging from individual to institutional size
packages (e.g., 6 kg sliced turkey breast package).
Batch, semi-continuous and continuous systems are
currently commercially available as HPP processing
equipment options. Continuous or semi-continuous HPP
systems are used only in a few cases to directly process
pumpable products, which then need to be aseptically
packaged. Batch processing that requires in-container pre-
packaged products is the most conventional of the three Fig. 1 Containers used for novel high-pressure products (Source:
operations and was relatively easy to implement in the food NC Hyperbaric 2010, personal communication)

123
276 Food Eng Rev (2010) 2:274–297

board–based packages are not recommended, as they HP-HT

deform irreversibly or tend to fracture under the com- T >100

f
pressive forces [6, 43]. When the treatment of packaging

Temperature (deg C)
T
materials is involved in the process, it is important to study T >70 dc
i
the safety of the material, the possible formation of com-
pounds that could influence the odor and taste of foods and
the effects of treatment on mechanical and physical prop-
erties of the packaging material, e.g., strength and barrier HP-LT
T
properties. f
T
High-pressure processing research and development in c
T T T
different disciplines within the food industry have been o o dc

extensively reviewed. However, no review has completed a HP-HT

combined study of the modern engineering aspects of HPP 680

technology and the packaging aspects of low- and high- 600

temperature applications in HPP food processing. More- HP-LT

over, the extensive progress made in recent years in HPP
processing merits a thorough review of these packaging
aspects. Consequently, this article addresses many of the
aspects associated with applying HPP as a processing
method in the food industry, from the fundamental physical
and heat transfer principles involved and requirements for
packaging, to the most recent analytical research methods
applied.
HPP Processing Cycle Food items are subjected to
pressures between 300 and 800 MPa. Pressurization of
compressible substances, such as a food product, results in
a temperature increase related to pressure increase. The
extent of this temperature rise depends on the pressure (P),
initial temperature (T0), and thermal and physical proper-
ties of the food and packaging. Pressure (P), temperature
(T), and time (t) are critical process parameters for estab-
lishing preservation process specifications to effectively
inactivate target pathogenic and spoilage microorganisms.
Commercial processing time can range from a few seconds
to over 20 min. The process temperature can range from
0 °C to temperatures higher than 100 °C. Pre-heating or
pre-cooling of products and temperature equilibration are
important steps in HPP to achieve the required process
temperature. Figure 2 schematically shows temperature
and pressure profiles during high pressure–low temperature
(HP-LT) and high pressure–high temperature (HP-HT)
processing utilized for pasteurization and sterilization,
respectively.
HPP Pasteurization and Sterilization Commercial HP–LT
processes achieve inactivation of vegetative microorgan-
isms at hydrostatic pressures of 600 MPa (or less) and
initial temperatures lower than 60 °C for 1–15 min
depending upon the product and process requirement [21].
Immediately after pressure release, the product temperature
returns to its initial value. The fast cooling capacity of HPP
is of most interest in the production of high-quality foods.
The use of lower temperatures has allowed better retention
Pressure (MPa)
Preheat CUT Holding CDT
8-10 min 2 min 3 min 1 min
Process time (min)
Fig. 2 Temperature and pressure histories during high-pressure
sterilization (HP–HT, solid line) and pasteurization (HP–LT, dotted
line) processes. Symbols represent product temperatures at initial
(T0), after preheat (Ti), during HP (Tf), after decompression (Tdc), and
after cooling (Tc) processes; CUT come-up time, CDT come-down
time
of sensory attributes characteristic of ‘‘fresh’’ or ‘‘just
prepared,’’ as well as food nutritional components [9]. As a
result, HP-LT has become a post-packaging technology
convenient for foods whose quality would otherwise be
altered by heat pasteurization.
As defined by US FDA, sterilization is a process to
remove or destroy all viable forms of microbial life,
including bacterial spores. HP–HT, also called pressure-
assisted thermal sterilization (PATS) or pressure-assisted
thermal processing (PATP), is an emerging preservation
method for the development of shelf-stable low-acid food
products and is a promising alternative to the conventional
thermal sterilization method [4]. This technique provides
fast heating and fast cooling due to hydrostatic compres-
sion and decompression, respectively, of the preheated
food package. In HP–HT sterilization, the volumetric
temperature increases to above 100 °C when using pres-
sures above 600 MPa, with a holding time of 3–5 min,
compared to 20–40 min in retort processing; this technique
has been shown to achieve microbial spore inactivation
[29]. Therefore, the reduced exposure of the product to
high temperatures can produce shelf-stable products with

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Food Eng Rev (2010) 2:274–297
sensory characteristics not achievable by conventional
retort processing [22, 38, 42]. For instance, pressurization
temperatures of 90–116 °C combined with pressures of
500–700 MPa for 3–5 min have been used to inactivate a
number of strains of C. botulinum spores [13, 40]. Other
researchers showed that certain bacterial endospores
(C. sporogenes, B. stearothermophilus, B. licheniformis,
B. cereus, and B. subtillis) in selected matrices including
phosphate buffer, beef, vegetable cream, and tomato puree
[3, 17, 31, 45, 52, 54] can be eliminated after short-time
exposure to temperatures and pressures above 100 °C and
680 MPa, respectively.
The critical parameters to establish pasteurization or
sterilization requirements are summarized in Table 1,
where products and HPP process parameters, target
microorganisms, packaging and conditions of storage
required in each case are compared.
Regulatory Status of HPP The US Food and Drug
Administration (FDA) and Department of Agriculture
(USDA) have approved HPP as a post-package pasteuri-
zation technology for manufacture of shelf-stable high-acid
foods and pasteurized low-acid food products and devel-
oped guidelines and regulations for those products (21CFR
§114 and 21CFR§113).
In 2009, the US FDA approved a petition for the com-
mercial use of PATS for application in the production of
low-acid foods, which has been filed for the first time for
processing in a 35-L high-pressure sterilization vessel.
Earlier, the European Commission on food regulations has
adapted existing legislation on novel foods to products
processed by HPP (EC258/97; [11]) and later on Health
Canada (Novel Food Decisions, available on Health
Canada’s website: http://www.novelfoods.gc.ca) issued
‘no-objections novel foods decisions’ concerning the ready-
to-eat meat and poultry products, which have been treated by
HPP for the control of Listeria monocytogenes (2006), as
well as for meat-containing entrees, meat-containing salads
Table 1 Critical product and
HP–LT
process conditions for
establishment of HPP Product parameters
preservation requirements
pH, aw 3.5 \ pH \ 4.6; pH \ 3.5
Process parameters
Temperature ( °C) B45
Pressure (MPa) B600
Target microorganisms
Pathogenic E. coli; Listeria; Salmonella
Spoilage Lactic bacteria, yeasts, molds
Storage Refrigerated conditions
Packaging Hermetically sealed flexible
containers
277
and meat products (2006), and applesauce and apple sauce/
fruit blends (2004).
Heat Penetration in Packages During Preheat Time
A preheating or temperature equilibration step is often used
to achieve the required initial temperature inside the
packages. However, package preheating can become a
limiting operation in the HP–HT sterilization process, since
it is related to the time required to reach a target temper-
ature at the geometrical center of the product before
pressure treatment. A rapid heat penetration rate is desir-
able for optimum process efficiency. A number of factors
influence the rate of preheating achieved in a product, such
as heating mode and system design, including the product
and container’s characteristics [24, 26]. In particular, the
thermal diffusivity of the packaging material (defined as a
ratio between the thermal conductivity and the product of
the density and heat capacity) affects the heat-penetration
rate according to the packaging material composition and
thickness. Other factors affecting the heat-penetration rate
of a package are the fill weight, the food package retaining
system (racks, trays, and cassettes), the container’s head-
space, the container’s shape, and the distribution of food
particulates.
The influence of the selected packaging materials on
heat-penetration rate within the product can be estimated
from time–temperature curves collected during the pre-
heating phase. The traditional parameters of heating rate
index fh (or time needed for a heat penetration curve to
cross one log cycle as -1/slope) and the heating lag factor
jh (Eq. 1) can be used to characterize the heat-penetration
rate for a specific type of packaging material.
 
ðTw  Ta Þ
jh ¼ ð1Þ
Tw  T0
where Tw is heating medium temperature, Ta is apparent
initial temperature needed to yield a straight line, and T0 is
HP–HT
pH [ 4.6; aw [ 0.86
[100
[700
C. botulinum spores
Geobacillus spp. Bacillus cereus
Ambient temperature
Hermetically sealed flexible
containers
123
278 Food Eng Rev (2010) 2:274–297

the initial temperature of the food. On the other hand, the
known heating rate index and heating lag factor can be
utilized to determine the time required to reach the target
preheat temperature Tb (tB, Eq. 2) inside the packaged
food.
 
jh ðTw  T0 Þ
tB ¼ fh log ð2Þ
Tw  Tb
Koutchma et al. [30] reported results of preheating trials
for ready-to-eat egg patties packed in two types of
laminated packages (polyethylene terephthalate/aluminum
foil/cast polypropylene (PET/Al/CPP), and biaxial poly
amide/coextruded ethylene–vinyl alcohol (BON/EVOH)
prior to HP–HT treatment. It has been shown that the
selected packaging material can affect the preheating rate
needed to achieve the target initial temperature, depending
on the composition and thickness of the material.
Physical Compression and Heat Transfer Behavior
of Packaged Foods During Pressurization
During pressurization, the packaged product undergoes
isostatic compression by the pressure-transmitting fluid,
causing a package volume reduction (compressibility) of
up to 19% depending on the final pressure and temperature
reached [6, 43, 56]. Table 2 shows the compressibility of
pure water at various temperatures. The pressure increase
inside the package is not only a result of mass augmenta-
tion from the pressure medium entering the chamber but
also due to shrinkage of the package under pressure.
In the package system, compression forces not only act
on the food materials, but also on the contained gas by
compressing it almost completely [43]. Food materials
nearly behave as water providing limited volume reduction.
Furthermore, compression forces act on the polymeric
materials forming the package, reducing the overall vol-
ume of food package. Once pressure is released, the food
package system undergoes a reversible or quasi-reversible
return to its initial volume. This may not apply to foods
with a porous structure (for example bakery goods) as they
Table 2 Compressibility (% volume reduction) of pure water at
various temperatures
Pressure (MPa) Compression ratio (%)
0 °C 50 °C 95 °C
0.1 0 0 0
100 4.3 3.7 3.9
200 7.5 6.7 7.1
400 12.1 11.1 11.6
800 – 16.9 17.5
1,000 – 19 19.7
may permanently shrink during compression. Flexible and
semi-rigid packaging are required because (a) they are
more resilient to the stresses induced by the high-pressure
compression forces and (b) they allow the instant pressure
transfer and compression of the headspace and food inside
the container [43, 56].
The compression effect on the plastic package volume
can be described with good approximation by the Tait
equation [6]:
lnðV=V0 Þ ¼ ln½1  C lnð1 þ P=CB0 Þ ð3Þ
where V0 and B0 are the polymer volume and the bulk
modulus at atmospheric pressure for each polymer,
respectively, P is pressure and C is a polymer-dependent
constant. Many polymers deform in a similar pattern,
irrespective of their chemical structure [55]. However,
polymers may decrease their volume with temperature/
pressure combinations [6]. Furthermore, the recovery of the
volume ratio of polymers after HPP might depend on the
temperature/pressure combination selected.
Fluids like air, water, and many food materials undergo
compression heating during pressurization and cooling
during decompression. In general, both the temperature of
the product and compression fluid may raise 20–40 °C
during HPP treatment. Solid metallic materials do not
experience significant compression heating. Therefore,
temperature increase may vary in foods with relatively
complex composition [49]. Water, carbohydrates, fats and
proteins are the main components of the complex food
matrix that respond uniquely under compression. It was
reported that water had the lowest temperature increase rate
under compression, about 3 °C/100 MPa at 25 °C, while
fats had the highest up to 6.7–8 °C per 100 MPa [1, 4, 51,
59]. As shown in Fig. 3, food components and other
polymeric materials provide variable compression heating
rates. Nevertheless, limited information is available on
compression temperature rise in real foods with complex
compositions.
In general, compression/decompression temperature
increases/decreases according to the pressure rate, nearly
linear (Fig. 3). Once the target temperature is fixed, a
constant compression rate should provide a constant com-
pression heating. However, as indicated by the compres-
sion heating equation (Eq. 4), this will depend on how the
volumetric expansion coefficient ap (1/K), the density q
(kg/m3), and the isobaric heat capacity Cp (J/kg K) of the
material will change during pressurization time [24] as well
as on the initial temperature T (K) of the material [5, 49].
dT Tap
¼ ð4Þ
dP qCp
Packaging materials also undergo compression heating.
Knoerzer and Versteeg [28] have shown that polypropylene

123
Food Eng Rev (2010) 2:274–297
(a) orange juice
Fig. 3 Temperature elevation from due to pressurization up to 700 MPa in various components: a orange juice [1] and b polymeric materials
[28]
(PP) and polyethylene (PE) undergo compression heating
greater than water under both HP–LT (10 and 50 °C) and
HP–HT (90 °C) conditions up to 750 MPa. In particular,
the temperature increase with pressure was not linear and,
therefore, the relative increase with respect to water
depended on the pressure range selected as well as the
initial temperature. For instance, PE showed higher
temperatures than water under both HP–LT and HP–HT
conditions throughout the whole pressure range. In
contrast, while temperature of PP remained higher than
that of water throughout the pressure range at HP–LT
conditions, the compression heating curve intersected with
water at 500 MPa at HP–HT conditions. Other authors
have observed a compression temperature increase of
4.5 °C/100 MPa on PP [56].
The decrease in polymer volume due to pressure
increase contributes to increased compression heating rate.
It has also been attributed to enhanced hydrophobic inter-
actions within the polymer structure [56]. Since under
adiabatic conditions the compression heating of the pack-
aging material may result in a higher temperature rise at
pressure than in both the food and compression medium, a
‘‘warmer’’ layer may be formed surrounding the food. This
phenomenon is an inherent part of the HPP process and
significant for chamber temperature if 5% of the vessel is
full of packaging material (assuming 5% in volume of
packaging material per food package) [23]. Determination
of the compression heating extent in different films would
help identify their influence on chamber temperature
homogeneity and inside the package.
In-Package Heat Loss Throughout the HPP Process Dur-
ing pressurization, the temperature of all matter contained
279
Water
(b) polymers
Propylene-Glycol
140 HDPE
PP
PTFE
120
100
Temperature (°C)
80
60
40
20
0
0 100 200 300 400 500 600 700
Pressure (MPa)
in the chamber increases temperature at different rates. This
includes each package (product, air and plastic/metal),
compression medium, and other inserts, which interact with
each other. Hence, it is important to consider how heat
transfer can affect temperature distribution throughout the
process due to the interaction of this matter. Even though in
a few cases packaging materials may assist in thermally
insulating the food during pressurization, this may not be
the main factor for heat retention during the HPP process. In
fact, the difference in compression temperature increase
between semisolid food and the vessel metal wall, where no
compression heating occurs, can be significant, and this
temperature difference can cause heat transfer out of the
food package. Consequently, ‘‘cold spots’’ or regions at
lower temperature can be located on the surfaces of pack-
ages near the vessel wall [24]. The package/vessel fill ratio
will determine the extent of temperature reduction inside
the total food mass being processed.
Computational fluid dynamic (CFD) models have been
developed to describe the temperature distribution of
packages contained inside the vessel during steps in the
high-pressure process [23]. Packages inside the vessel were
shown to act as a barrier to flow and heat, preventing the
cooling down from the incoming ‘‘colder’’ pressurization
fluid. However, lack of wall insulation results in colder
areas near the vessel walls, while higher temperatures
remain in those packages that are located at the center of
the vessel [20]. Other simulations from [19, 20] suggested
that polypropylene (PP) packages with smaller heat trans-
fer coefficients (lower thermal conductivity to thickness
ratio) contained in a 50-L vessel retain more heat than
similar packages contained in a laboratory scale 0.8-L
123
280 Food Eng Rev (2010) 2:274–297

vessel. In the smaller vessel, the package boundaries are
closer to the vessel walls and the fluid inlet. In contrast,
another CFD model of a 35-L HP sterilization vessel
included an insulating polymeric polytetrafluoroethylene
(PTFE) carrier in contact with the vessel walls and upper
vessel lid. PE packages placed inside the carrier with a
‘‘water-like’’ simulant showed that the end temperature
inside the packages was not affected during the processing
[25, 27].
Requirements for HPP Packaging Materials
A number of requirements that define the packaging
integrity and barrier properties must be met during and
after processing. In this way, the package can allow the
preservation of the HPP-treated food qualities throughout
its shelf life.
Flexibility
As previously indicated, HPP packaging material must
have sufficient flexibility and resilience to withstand the
operating pressures and to retain its integrity, barrier
properties, and strength properties (Table 3). Metal or
inorganic coatings on films can create an unreliable
structure due to barrier loss resulting from compression
damage to the inorganic barrier layer [44].
Visual Integrity
The package should maintain its visual integrity by
avoiding delamination, creasing, pinholes, crazing, or other
pressure-induced defects. Delamination not visible to the
naked eye should also be assessed when developing a HPP-
specific packaging material.
Gas Barrier
Requirements for gas barrier properties depend on the
product application and intended storage temperature.
Industrial norms allow up to 12% deviation from standard
oxygen and water barrier levels [34]. For developing shelf-
stable products to be stored above room temperature, the
US army has specified a 0.06 mL/m2/day oxygen perme-
ability limit and a 0.01 g/m2/day water permeability limit.
These specifications are required for a shelf life of 3 years
at 25 °C or 6 months at 37 °C. On the other hand, some
commercial shelf-stable products require an oxygen per-
meability value between 0.1 and 0.2 mL/m2/day. Retort
pouches generally carry a middle Al layer (e.g., 7, 9, and

Table 3 General requirements for pouches acceptable for HPP and retort
Integrity requirementa (maximum HP–LT (600 MPa/80 °C) HP–HT (800 MPa/133 °C) Retortb (0.2 MPa/133 °C)
expected pressure/temperature)

Visual integrity No delamination or blistering No delamination or No delamination or blistering

blistering
Oxygen permeability Product dependent 0.06 for US military or 0.06 for US military or
(maximum deviation 12%) 0.5–1.0 mL/m2/day for 0.5–1.0 mL/m2/day for some
some commercial commercial products
products
Water permeability Product dependent 0.01 g/m2/day or product 0.01 g/m2/day or product
(maximum deviation 12%) dependent dependent
Seal strength properties Material dependent Material dependent Seal strength, 2–3.5 kg/100 mm;
(maximum deviation 25%) bond strength 150–500 g/10 mL;
burst test 7.5 kg/15 mm seal
Physical strength (tensile, Material dependent Material dependent Material dependent
elongation, elasticity modulus;
maximum deviation 25%)
Global migration of packaging \10 mg/dm2 \10 mg/dm2 \10 mg/dm2
components to food simulantsc
Maximum headspacea,d Up to 30% Up to 30% Up to 30%
d
High thermal conductivity Not required Required Required
(with exceptions)
a
Lambert et al. [33, 34]. Headspace requirement as per Japanese standard
b
Venugopal [60]
c
EU 90/128
d
Not yet defined as a standard selection criterion

123
Food Eng Rev (2010) 2:274–297
15 lm thick), which functions as a moisture, light, and gas
barrier [60].
Material and Seal Strength
Retention of strength properties of a material refers to its
tensile strength and the seal strength. Furthermore, the
elastic modulus and the percentage of elongation can assess
the deformation of the package after processing [7].
Industrial norms suggest that deviations in tensile strength,
elongation, elasticity modulus, as well as seal strength,
must remain within the 25% range for these properties [34].
Physical strength must be high enough to provide the
mechanical strength (puncture resistance) to withstand
handling during manufacturing and distribution. For
example, retort pouches contain an outer layer of PET (e.g.,
12 lm thick), which gives the pouch strength, abrasion
resistance, and a surface for printing labeling information.
The inner food-contact material layer (e.g., 50–70 lm PP)
provides the heat seal strength. In general, hot bar sealing is
preferred to impulse sealing. A double sealing of 5–10 mm
per sealing area is desired for good strength and to reduce
the risk of seal defects [60].
Headspace
In order to prevent unnecessary stress over the package, the
headspace must be minimized while sealing the package.
This will also maximize utilization of the vessel capacity
and minimize the time needed to reach the target process
pressure and temperature. A maximum headspace of 30%
has been recommended [33]. Typically an HPP vessel will
utilize its 50–70% volume capacity depending on the shape
of the package and the vessel design [34]. If the HPP
process requires preheating of the food product, the highest
possible thermal conductivity is desirable for the material.
Furthermore, the melting point and glass transition tem-
perature of polymers should be considered when selecting
a polymer for HPP to maintain dimensional stability of the
packages [60].
Aging and Printability
Additional desirable properties of packaging polymers
include good aging properties and printability [60]. The
material must also not allow the migration of compression
fluid or food components through the package or the
transfer of packaging components to the food during pro-
cessing or storage. Section ‘‘Migration and Sorption of
Packaging and Food Components’’ summarizes the litera-
ture published in this area.
281
Barriers for Flexible and Semi Rigid Packaging
High-pressure processing enables treatment of food sealed
in multiple ready-to-use containers or in larger bulk
packages for stabilization. After HPP treatment, the pack-
aging material must retain some target barrier to oxygen,
moisture and light in order to achieve desired shelf life and
to limit detrimental chemical or enzymatic reactions
mainly caused by presence of oxygen and exposure to light.
Barrier functionality can be obtained either by adding a
layer of barrier material or by mixing the barrier material
into the bulk polymer [36]. Pouches traditionally contain a
layer of aluminum or some high barrier polymers such as
poly(vinylidene chloride) (PVDC), EVOH, poly(vinyl
alcohol) (PVOH) or nylon (often identified generically as
polyamide, PA). Aluminum has also been used as a foil
layer a few micrometers thick or a metalized vacuum-
deposition coating with a thickness in the nanometer range.
An Al foil sheet provides an excellent barrier to oxygen,
light and moisture except where cracks, pinholes, or other
imperfections are present in the foil layer. Metalized layers
can provide good barriers at a lower cost. High barrier
layers can be integrated into packaging structures either by
coextrusion or lamination. Most high oxygen barrier
polymers (e.g., PVOH, EVOH and most PAs) are good
barriers when dry, therefore must be sandwiched between
water vapor barrier films such as PET and PE to maintain
their full oxygen barrier functionality. Table 4 presents the
permeability of some commonly used polymers and cur-
rently available flexible films with barrier layers [36].
Retortable pouches have also been developed as a
packaging alternative to cans for low-acid foods by means
of thermal processing. These types of pouches are com-
monly made of 4-ply layers of PET and PE or PET/PA/Al/
retortable CPP laminated with polyurethane adhesive.
Microwavable options use an AlOx-PET/PA/retortable CPP
structure. Some pouch material uses PVDC, EVOH, or PA
instead of Al as the middle layer to permit viewing the
product [50]. However, moisture migration at retort tem-
perature can compromise the oxygen barrier. These types
of pouches have been also evaluated as packaging for HP–
HT processing, as will be shown in the following section.
Table 5 provides a list that summarizes the container
types commercially utilized for various product applica-
tions (fruits and vegetables, red meat and poultry, fish, and
dairy) by a number of companies in Australia, Germany,
New Zealand, and the USA. These are products of HPP
utilizing low temperature including refrigerated ready to
eat meals. In this case, single and combinations of PET,
PE, PP and EVOH are common materials composing trays,
bottle, and flexible pouches. Stand up and resealable pou-
ches are becoming a popular option for high value addition
in HPP applications.
123
282 Food Eng Rev (2010) 2:274–297

Table 4 Permeability of
Polymer Oxygen permeability Water vapor permeability
polymers commonly used in
at 23 °C 50% at 23 °C 85%
packaging [60]
or 0% RH (mL/m2/day) RH (g/m2/day)

Ethylene vinyl alcohol (EVOH) 0.001–0.01 (dry) 1–3

Poly(vinylidene chloride) (PVDC) 0.01–0.3 0.1
Poly(vinyl alcohol) (PVAL) 0.02 (dry) 30
Polyamide (PA) or nylon 0.1–1 (dry) 0.5–10
Poly(ethylene naphthalate) (PEN) 0.5 0.7
Poly(ethylene terephthalate) (PEF) 1–5 0.5–2
Poly(vinyl chloride) (PVC) 2–8 1–2
Polypropylene (PP) 50–100 0.2–0.4
Polyethylene (PE) 50–200 0.5–2
Polystyrene (PS) 100–500 1–4

Table 5 Commercial HPP packaging by product applications (NC Hyperbaric 2010, personal communication)
Product type Product Packaging description Materials Example

Fruits & Fruit and vegetable Bottle with screwed PETE, PE PET bottle from Preshafruit
vegetable juices caps in few cases with (Australia)
sealed metalized top
foil
Tomato salsa Cup with sealed top film PETE (cup) Pouch from SimplyFresco
and stand-up (USA)
resealable pouches
(SURP)
Guacamole Cup and top sealable PP (cup) Vacuum packed bag from
film and vacuum fresherized foods (USA)
packed pouch
Meat Small cooked pork Preformed tray and top Darfresh from Cryovac Espuña ready to eat tapas
sausages, sliced skin film
blood sausages
Cooked sliced Skin pack (combined Upper film: PS-EVOH MRM (Spain)
meats, sliced film at top and Bottom film: PE-EVOH
bacon, sliced pork bottom)
Or
meat, small
sausages Upper film: PE
Bottom film: PP
Whole prosciutto Vacuum pack metalized PET/Metal/LLDPE or Abraham Schinken GmbH
bag PET/Metal/Nylon (Germany)
Sliced prosciutto Modified atmosphere Bottom film: A-PET/PE Abraham Schinken GmbH
packaging (PEEL) (Germany)
Top film: PET/PE or
BOPP/PE or
BOPP/PET/PE)
Sliced cooked Zip re-sealable vacuum Oscar Mayer (USA)
poultry pack bag
Fish Ready-to-eat fish Preformed tray and top RTE fish meal from MRM
meals with sauce skin film (Spain)
Dairy Sandwich spreads Tray with sealed top PET (tray and top) Tray & flexible pouches
and other (fresh cheese and film and top flexible from Rodilla (Spain)
mayonnaise based) pouch
Colostrum Bottle including foil HDPE and foil New image group (New
Zealand)

123
Food Eng Rev (2010) 2:274–297
Overall Packaging Integrity After HPP
High-pressure processing can alter integrity of multilay-
ered materials including adhesion between layers. Adhe-
sion between layers can be compromised if compressibility
and resilience of individual layers differ significantly. The
resulting gaps between the layers may even affect the
microbiological safety of the package [8].
The previous section listed a number of requirements
that packaging materials need to meet in order to provide
adequate protection to the food throughout storage. Among
those, physical and visual integrity, oxygen and water
permeability, and mechanical strength have been selected
as a first screening criterion to assess the performance of
packaging listed in the literature. A classification has been
done between packages processed at HP–LT conditions
(i.e., equal or below 60 °C initial processing temperature)
and HP–HT conditions (i.e., above 60 °C initial processing
temperature).
Tables 6 and 7 classify packaging materials processed
at HP–LT and HP–HT conditions, respectively. Each
table groups the materials according to the main barrier
component where applicable (i.e., EVOH, PVDC, PA,
SiOx, Al-based and metalized, PE, PET, and others). The
information summarized in the tables is sufficient to
reject certain packages based on the main properties lis-
ted. However, additional information is needed to provide
the full picture of the readiness of the packages. For
example, the diffusion of packaging material components
into the food as well as the migration of food compo-
nents (or pressure medium) through the material requires
closer consideration to be utilized as selection criteria.
Furthermore, microscopic analysis performed to deter-
mine material integrity (i.e., delamination at the
micrometer level) can be of assistance during the pack-
aging selection. However, not meeting gas permeability
and strength property requirements is sufficient for initial
rejection and out-screening. In some cases, the perme-
ability values of packages evaluated before HPP were
already problematically high, making their deviation after
HPP irrelevant.
Overall Packaging Integrity After HP–LT
By summarizing the results of reported studies (Table 6), it
can be concluded that most EVOH-based packaging treated
at HPP and initial temperature lower or equal to 60 °C
retained visual and physical integrity, showing no signs of
delamination. In general, oxygen and water permeability
after HPP fitted within the specified deviation limits
(within 12% deviation according to industrial norms). In
some cases, HPP acted beneficially by mildly decreasing
283
both oxygen and water permeability. However, not all the
EVOH-based materials tested had low oxygen permeability
before HPP. For example, the oxygen permeability level
for the EVOH48-based package [39] initially carried a
much higher value (48 mL/m2/day) than the EVOH26-
based packages (under 5 mL/m2/day). Material and seal
strength properties of EVOH-based packages, where
reported, underwent minor deviations after pressure (under
25% as required by industrial norm).
The visual integrity of four PVDC-based materials was
not greatly affected by HP–LT processing. Only a combi-
nation of PET/PVDC/PA/HDPE/PP showed small wrinkles
and signs of delamination or wear on the PP side after an
800 MPa and 45 °C treatment [7]. The oxygen perme-
ability in all PVDC-based materials remained within the
original value. The water permeability of the PET/PVDC/
PE material [33] increased by 109% (outside the 12%
criterion) after 500 MPa and 20 °C. However, PVDC-
based materials cannot be rejected outright because values
obtained after HP–LT processing are comparable to those
of other PVDC-based materials listed in Table 6. These
materials were not changed after HP–LT. The tensile
strength of the PET/PVDC/EVA/LLDPE material [7] was
reduced by 63% (outside the 25% industrial deviation).
However, this composite provided a tensile strength com-
parable to the PET/PVDC/PE [37]. The latter structure, like
other PVDC-based structures tested by other authors
(Table 6), showed no deviation of tensile strength,
although the seal strength of these materials should be
compared under equal conditions.
Even though about ten PA-based materials were tested,
little has been reported on their visual integrity after HP–
LT processing. In a PA/PE composite, delamination seems
to be affected by the thickness of each layer [33]. After
HP–LT, an increase by more than 12% in oxygen perme-
ability was reported for a few PA-based packages
(Table 6). In terms of water permeability after HP–LT,
results were variable and depended on the composition,
thickness and number of layers, as well as method of
fabrication (supplier). In general, the PA barrier provides
higher oxygen permeability values than EVOH and PVDC
(Table 4); however, the required oxygen permeability will
depend on the product application. In addition, the barrier
properties of the EVOH and nylon (PA) materials are best
when dry. Even though PA is used for its toughness rather
than barrier properties in some structures, these structures
may be unsuitable for HPP. High barrier grades of PVDC
are more brittle than EVOH and nylons and may undergo
stress fracturing when HPP treated.
Interestingly, a general increase has been seen in tensile
strength after HP–LT (by up to 39%), whereas no signifi-
cant changes (with some exceptions seen over the industry-
acceptable 25% limit) have been observed in seal strength.
123
 284

Table 6 Overall appearance (visible integrity, delamination), permeability and strength properties of films tested at HPLT conditions. Percentages indicate variation with respect to the
control*

123
Test film structure Thickness Manufacturer Max pressure/ Physical/visual Oxygen Water Tensile strength Elongation Elastic modulus Seal strength References
(lm) time/initial temp. integrity permeability permeability (control c.d., MPa) (control c.d., %) (control c.d., MPa) (control c.d. (N/
(MPa/min/ °C) (delamination) (control) % post (control) % post % post HHP % post HHP % post HHP 15 mm)) % post
HHP HHP HHP

EVOH-based
LLDPE/EVA/EVOH/ n/a Pira 400/30/60 Retained (0.74) - 15% (1.9) - 5% (27 N) ? 1% (530.0) ? 0% n/a (?) ? 0% Mertens [43]
EVA/LLDPE
LDPE/EVOH/LDPE/ 500 Wipak 600/60/20 n/a n/a (0.92)0% (70.1) ? 5% n/a n/a (82.6) ? 0% Dobias et al.
APET/Exp. PET/ [10]
APET
PE/PA/EVOH/PE 140 Wipak 600/60/20 n/a n/a (6.0) - 5% (58.3) ? 0% n/a n/a (52.7) ? 8% Dobias et al.
[10]
PE/EVOH/PE 53/12/53 n/a 400/30/20 n/a n/a ? (44.2) ? 13% (436.5) ? 19% n/a n/a Galotto et al.
[15]
PE/EVOH/PE 53/12/53 n/a 400/30/60 n/a n/a ? (44.2) ? 6% (436.5) ? 6% n/a n/a Galotto et al.
[15]
PA/PE/EVOH/PE n/a n/a 550/20/55 Retained (2 - 3)0% n/a n/a n/a n/a n/a Moueffak
coextruded et al. [47]
PET/PE/EVOH/PE 60 Wipak 600/60/20 n/a n/a (8.8) ? 3% (57.2) ? 5% n/a n/a (65.3) - 9% Dobias et al.
[10]
PE/nylon/EVOH/PE 62.5 Cryovac 800/20/45 Retained (*2) ? 2% (*23) ? 1% (20.4) - 18% (529.6) ? 2% (344.4) ? 1% n/a Caner et al.
[7, 8]
PP/EVOH/PP 35/10/60 Nippon 600/10/20 Retained (4.8) ? 10% (5.2) ? 15% (3.3) - 3% n/a n/a (3.3) ? 3% Masuda et al.
Synthetic [41]
Chemical
Industry
PA/PP/EVOH/PP n/a n/a 550/20/55 Retained (white (3–4) variable n/a n/a n/a n/a n/a Moueffak
coextruded stains) et al. [47]
PP/EVOH26/PP 100/10/ Nippon 800/10/40 Retained (0.6) - 2% n/a n/a n/a n/a n/a Lopez-Rubio
coextruded 100 Synthetic et al. [39]
(w adhesive) Chemical
Industry
PP/EVOH48/PP 100/10/ Nippon 800/10/40 Retained (40.9) - 7% n/a n/a n/a n/a n/a Lopez-Rubio
coextruded 100 Synthetic et al. [39]
(w adhesive) Chemical
Industry
PVDC-based
PET/PVDC/nylon/ 102.5 Rexam Inc. 800/20/45 Retained (*2) ? 2% (*3) ? 1% (66.5) ? 15% (106.7) ? 0% (558.0) ? 5% n/a Caner et al.
HDPE/PP [7, 8]
PET/PVDC/EVA/ 50 Cello-Foil Pro 800/20/45 Retained (small (*3) ? *9% (*23) ? 14% (55.5) - 63% (535.0) ? 6% (336.5) ? 1% n/a Caner et al.
LLDPE Inc. wrinkles on food [7, 8]
contact side)
PET/PVDC/PE 65 Soplaril 600/10/10 n/a n/a (5.79) - 1% (39.2) ? 4% (36.1) ? 0% n/a n/a Le-Bail et al.
[37]
Food Eng Rev (2010) 2:274–297
 Table 6 continued
Test film structure Thickness Manufacturer Max pressure/ Physical/visual Oxygen Water Tensile strength Elongation Elastic modulus Seal strength References
(lm) time/initial temp. integrity permeability permeability (control c.d., MPa) (control c.d., %) (control c.d., MPa) (control c.d. (N/
(MPa/min/ °C) (delamination) (control) % post (control) % post % post HHP % post HHP % post HHP 15 mm)) % post
HHP HHP HHP

PET/PVDC/PE free (12/1/ Soplaril- 500/30/20 Retained (11) ? 10% (3.5) ? 109% (347.0) ? 8% n/a n/a (3.5) ? 6% Lambert et al.
radical, linear 50)65 Sodap [34]
PA (nylon)-based
Food Eng Rev (2010) 2:274–297

Nylon/PP n/a The Pyramid 600/3/5 Retained (blisters?) (8.9) ? 17,700% n/a n/a n/a n/a n/a Koutchma
Group, La et al. [30]
Habra, CA
PA/PE free radical, (30/ Soplaril- 500/30/20 Retained (66) ? 2% (5.9) - 25% (149.8) ? 32% n/a n/a (3.8) - 8% Lambert et al.
linear 60)100 Sodap [34]
PA/PE free radical, (40/ Soplaril- 500/30/20 Delamination n/a n/a (162.8) ? 39% n/a n/a (3.95) - 24% Lambert et al.
linear 40)100 Sodap [34]
PA/PE (40/ RC302 500/30/20 Retained (62) - 16% (10.5) - 47% (192.2) ? 19% n/a n/a (3.5) ? 4% Lambert et al.
surlyn:ionomer Zn 55)110 Soplaril- [34]
Sodap
PA/MDPE (20/ Soplaril- 500/30/20 Retained (68) ? 26% (3.5) ? 24% (177.5) ? 16% n/a n/a (2.6) - 6% Lambert et al.
70)100 Sodap [34]
PA/PE extruded 100 Soplaril 600/60/20 n/a n/a (0.64) ? 29% (37.5) ? 0% n/a n/a (40.6) ? 0% Dobias et al.
[10]
PA/PE 90 Vacopack 600/60/20 n/a n/a (0.93) ? 12% (25.6) ? 25% n/a n/a (32.9) ? 139% Dobias et al.
[10]
PA/PE 80 Chemosvit 600/60/20 n/a n/a (1.02) ? 60% (21.1) ? 7% n/a n/a (25.1) ? 0% Dobias et al.
[10]
NOD 259 (PA-PE) 59 Cryovac 600/10/10 n/a n/a (67.1) - 1% (30.1) ? 8% (41.2) ? 0% n/a n/a Le-Bail et al.
[37]
PA/surlyn 180 Soplaril 600/10/10 n/a n/a (4.76) - 1% (29.2) - 6% (343.6) ? 0% n/a n/a Le-Bail et al.
[37]
PP/nylon/PP 115 Rexam Inc. 800/20/45 Retained (*5) ? *10% (*5) ? *2% (57.2) - 7% (63) ? 8% (457.5) ? 0% n/a Caner et al.
[7, 8]
PE/nylon/PE 50 Cryovac 800/20/45 Retained (*95) ? 5% (*16) ? 2% (23.3) ? 125% (126.2) ? 6% (364.0) - 3% n/a Caner et al.
[7, 8]
PE/PA/PE n/a n/a 550/20/55 Retained (25 - n/a n/a n/a n/a n/a Moueffak
35) ? 60% et al. [47]
PE/PA/PE (foie gras) n/a n/a 400/20/50 Retained (35 - n/a n/a n/a n/a n/a Moueffak
40) ? 91% et al. [46]
LDPE/PA/LDPE 100 Aliachem 600/60/20 n/a n/a (1.5) ? 7% (40.8) ? 8% n/a n/a (41.7) - 17% Dobias et al.
[10]
PA/PP/PE free radical, (30/10/ KL174 500/30/20 Retained (103) ? 2% (4.1) ? 15% (187.1) - 9% n/a n/a (2.7) - 9% Lambert et al.
linear 60)110 Soplaril- [34]
Sodap
285

123
 286

Table 6 continued
Test film structure Thickness Manufacturer Max pressure/ Physical/visual Oxygen Water Tensile strength Elongation Elastic modulus Seal strength References

123
(lm) time/initial temp. integrity permeability permeability (control c.d., MPa) (control c.d., %) (control c.d., MPa) (control c.d. (N/
(MPa/min/ °C) (delamination) (control) % post (control) % post % post HHP % post HHP % post HHP 15 mm)) % post
HHP HHP HHP

SiOx-based
PP/SiOx 21 n/a 400/30/20 Delamination n/a ? (18.8) ? 114% (5.9) ? 98% n/a n/a Galotto et al.
(mechanical [15]
properties
affected)
PP/SiOx 21 n/a 400/30/60 Delamination n/a ? (18.8) ? 251% (5.9) ? 756% n/a n/a Galotto et al.
(mechanical [15]
properties
affected)
PET/SiOx/LDPE 62.5 GL-AE 800/20/45 Retained (small (1.6) ? 11% (*4) ? 9% (48.8) - 14% (153.9) ? 2% (373.7) ? 4% n/a Caner et al.
Toppan Co. wrinkles on food [7, 8]
Al-based or metalized
PET/Al/CPP 09/12/ Nippon 600/10/20 Retained (0.3)0% (0)0% (5.0) - 4% n/a n/a (4.6) - 7% Masuda et al.
1970 Synthetic [41]
Chemical
Industry
PET/Al/PP n/a Pira 400/30/60 Retained (0.38) - 71% (0.04) - 25% (62 N) ? 1% (80.0) ? 9% n/a (?) ? 0% Mertens [43]
PET/Al/PE n/a n/a 550/20/55 Damaged (heat 0% n/a n/a n/a n/a n/a Moueffak
seals broken) et al. [47]
PET/Al/LDPE 62.5 GL-AE 800/20/45 Retained (small (1.6) ? 11% (*4) ? 11% (49.7) - 18% (157) ? 3% (374.8) ? 1% n/a Caner et al.
Toppan Co. wrinkles on food [7, 8]
contact side)
PETmet/VA EVA/ 50 Cello-Foil Pro 800/20/45 Damaged (fold and (*3) ? 95% (*7) ? 150% (63.8) - 14% (140.9) ? 0% (322.1) - 5% n/a Caner et al.
LLDPE Inc. wrinkles on food [7, 8]
contact layer)
PETmet/PE 75/19 n/a 400/30/20 Delamination n/a ? (57.1) ? 4% (44.2) - 7% n/a n/a Galotto et al.
[15]
PETmet/PE 75/19 n/a 400/30/60 Delamination n/a ? (57.1) ? 3% (44.2) - 17% n/a n/a Galotto et al.
[15]
PE-based
LDPE (commonly 202 EM2 600/10/10 n/a n/a (71.2) - 1% (9.0) - 2% (299.3) ? 0% n/a n/a Le-Bail et al.
used for HPLT) [37]
PE 2686 50 Aliachem 600/60/20 n/a n/a (2.8)0% (18.4) ? 5% n/a n/a (14.6) - 42% Dobias et al.
(LDPE ? LLDPE) [10]
PE Granoten LM1A 70 Granitol 600/60/20 n/a n/a (1.9)0% (25.1) ? 0% n/a n/a (2.5) - 52% Dobias et al.
(LDPE ? LLDPE) [10]
PET-based
PET/PE 93/17 n/a 400/30/20 n/a n/a ? (68.4) ? 5% (44.6) - 8% n/a n/a Galotto et al.
[15]
PET/PE 93/17 n/a 400/30/60 n/a n/a ? (68.4) - 8% (44.6) - 17% n/a n/a Galotto et al.
[15]
Food Eng Rev (2010) 2:274–297
 Table 6 continued
Test film structure Thickness Manufacturer Max pressure/ Physical/visual Oxygen Water Tensile strength Elongation Elastic modulus Seal strength References
(lm) time/initial temp. integrity permeability permeability (control c.d., MPa) (control c.d., %) (control c.d., MPa) (control c.d. (N/
(MPa/min/ °C) (delamination) (control) % post (control) % post % post HHP % post HHP % post HHP 15 mm)) % post
HHP HHP HHP

PP-based
PP antifog 30 Aliachem 600/60/20 n/a n/a (3.5) ? 0% (17.6) ? 7% n/a n/a (5.0) - 52% Dobias et al.
[10]
PP cast unoriented 40 Aliachem 600/60/20 Total loss of n/a (2.4) ? 6% (20.5) ? 4% n/a n/a Total loss of Dobias et al.
sealability sealability [10]
Food Eng Rev (2010) 2:274–297

BOPP 40 Aliachem 600/60/20 n/a n/a (2.6)0% (31.0) ? 7% n/a n/a (3.2) ? 0% Dobias et al.
[10]
KOP/CPP 20/40 Nippon 600/10/20 Retained (11) ? 10% (3.4) ? 12% (6.4) - 5% n/a n/a (3.3) - 3% Masuda et al.
Synthetic [41]
Chemical
Industry
Others
OPP/PVOH/PE 20/12/40 Nippon 600/10/20 n/a (0.3)0% (2.9) ? 10% (8.6) - 8% n/a n/a (4.7) ? 9% Masuda et al.
Synthetic [41]
Chemical
Industry
Surlyn 1605 60 Du Pont 600/60/20 n/a n/a (2.7)0% (23.6) ? 0% n/a n/a (4.6) ? 313% Dobias et al.
(copolymer of [10]
ethylene and
methacrylic acid)
Surlyn 8140 75 Du Pont 600/60/20 n/a n/a (2.4) ? 7% (32.2) ? 0% n/a n/a (20.0) ? 0% Dobias et al.
(copolymer of [10]
ethylene and
methacrylic acid)
EVA/PE 50 Prochimir 600/10/10 n/a n/a (93.1) - 1% (14.6) ? 5% (393.4) ? 0% n/a n/a Le-Bail et al.
[37]
BB4L (internal PE) 59 Cryovac 600/10/10 n/a n/a (25.3) ? 16% (33.7) ? 4% (67.7) ? 2% n/a n/a Le-Bail et al.
[37]
PET/BOA/PE 62 Soplaril 600/10/10 n/a n/a (6.05) ? 9% (28.7) - 4% (41.3) ? 0% n/a n/a Le-Bail et al.
[37]

* ?12% allowed deviation from untreated in oxygen (mL/m2/day) and water vapor barrier (g/m2/day) permeability and 25% deviation in tensile strength and seal strength as per Soplaril industrial norms [34]. n/a indicates information
not available
287

123
 288

123
Table 7 Overall appearance (visible integrity, delamination), permeability and strength properties of films tested at HPHT conditions*
Test film structure Thickness Manufacturer Max pressure/ Physical/visual Oxygen Water Tensile Elongation Elastic Seal strength References
(lm) time/initial integrity permeability permeability strength (control c.d. modulus (control c.d. (N/
temp. (MPa/ (delamination) (control) % post (control) % (control c.d., %) % post (control c.d., 15 mm)) % post
min/ °C) HHP post HHP MPa) % post HHP MPa) % post HHP
HHP HHP

EVOH-based
Biaxial PA/ 144 Alcan, 688/3/88 Retained (0.05) ? 3,900% n/a n/a n/a n/a (409.4)-13% Koutchma
coextruded Minneapolis, et al. [30]
EVOH MN
PA/EVOH/PE 75 Winpak 690/10/95 Retained n/a n/a n/a n/a n/a n/a Schauwecker
(Deli*1) et al. [56]
PE/PA(Nylon6)/ (28/13/8/ Pliant Corp. 800/10/70 n/a (1) - 50% (5.5) ? 9% n/a n/a n/a n/a Halim et al.
EVOH/PE 17/ Schaumburg, [18]
34)100 IL, USA
PP/EVOH26/ 100/10/ Nippon 800/10/75 Retained (0.6) - 2% n/a n/a n/a n/a n/a Lopez-Rubio
PPcoextrud ed 100 Synthetic et al. [39]
(w adhesive) Chemical
Industry
PP/EVOH48/PP 100/10/ Nippon 800/10/75 Retained (40.9) - 7% n/a n/a n/a n/a n/a Lopez-Rubio
coextruded 100 Synthetic et al. [39]
(w adhesive) Chemical
Industry
PA/PE/EVOH/PE n/a n/a 550/20/85 Retained (2–3)0% n/a n/a n/a n/a n/a Moueffak
coextruded et al. [47]
PA/PP/EVOH/PP n/a n/a 550/20/85 Retained (3–4)variable n/a n/a n/a n/a n/a Moueffak
coextruded (white stains) et al. [47]
PA (nylon)-based
PA/PP n/a The Pyramid 688/3/88 Retained (8.9) ? 45,100% n/a n/a n/a n/a (309.9)-13% Koutchma
Group, La (blisters) et al. [30]
Habra, CA
PE/PA(Nylon6)/PE (28/45/ Pliant Corp. 800/10/70 n/a (15.2) ? 15% (5.5) ? 7% n/a n/a n/a n/a Halim et al.
27)100 Schaumburg, [18]
IL, USA
PE/ (36/27/ Pliant Corp. 800/10/70 n/a (4.1) ? 46% (4.7) ? 17% n/a n/a n/a n/a Halim et al.
PA(Nylon6Nano)/ 37)100 Schaumburg, [18]
PE IL, USA
PE/PA/PE n/a n/a 550/20/85 Retained (25–35) ? 60% n/a n/a n/a n/a n/a Moueffak
et al. [47]
Food Eng Rev (2010) 2:274–297
 Table 7 continued
Test film structure Thickness Manufacturer Max pressure/ Physical/visual Oxygen Water Tensile Elongation Elastic Seal strength References
(lm) time/initial integrity permeability permeability strength (control c.d. modulus (control c.d. (N/
temp. (MPa/ (delamination) (control) % post (control) % (control c.d., %) % post (control c.d., 15 mm)) % post
min/ °C) HHP post HHP MPa) % post HHP MPa) % post HHP
HHP HHP

Al-based or metalized
PA/Al/PP n/a The Pyramid 688/3/88 Retained (0.05) ? 780% n/a n/a n/a n/a (360.8)?75% Koutchma
Group, La (blisters) et al. [30]
Habra, CA
Food Eng Rev (2010) 2:274–297

PE/PA/Al/PP 142 Smurfit-Stone 690/10/90 Delamination n/a n/a n/a n/a n/a n/a Schauwecker
(no et al. [56]
delamination
at T \ 90 °C)
PET/Al/PE n/a n/a 550/20/85 Damaged (heat 0% n/a n/a n/a n/a n/a Moueffak
seals broken) et al. [47]
PET/Al/CPP n/a Smurfit-Stone, 688/3/88 Retained (0.05) ? 700% n/a n/a n/a n/a (185.6)?31% Koutchma
Schaumburg, (blisters) et al. [30]
IL
PET/AlOx/CPP n/a Toppan Co., 688/3/88 Retained (0.05) ? 39,100% n/a n/a n/a n/a (53.6)?55% Koutchma
Japan et al. [30]
Others
PET/PE n/a Ampac 688/3/88 Retained (78.2) - 68% n/a n/a n/a n/a n/a Koutchma
Flexibles et al. [30]
Corporation,
Minneapolis,
MN
PEF/PE n/a n/a 695/10/70 White opaque n/a n/a n/a n/a n/a n/a Fairclough
area and lines and Conti
[12]

* 12% allowed deviation from untreated in oxygen (mL/m2/day) and water vapor barrier (g/m2/day) permeability and 25% deviation in tensile strength and seal strength as per Soplaril industrial norms [34].
n/a indicates information not available
289

123
290
The two SiOx-based materials tested [7, 15] showed
visual integrity problems due to delamination (PP/SiOx) or
formation of small wrinkles on the food contact side (PET/
SiOx/PE). Oxygen and water permeability increased for the
PET/SiOx/PE laminate. However, the change remained
under the 12% acceptable limit after HP–LT, showing a
durability of the outer PET/SiOx layers to HP–LT treat-
ment. While PET/SiOx/PE maintained strength properties,
the strength of PP/SiOx was increased by more than 100%
after HP–LT (Table 6).
Three out of seven tested metal-foil materials (Table 6),
PET/Al/CPP (Nippon), PET/Al/PP (manufacturer not
reported), and PET/Al/LDPE (Toppan) survived the
HP–LT process without significant delamination [7, 41,
43]. However, a similar material to the PET/Al/PE (man-
ufacturer not reported) did not retain seal integrity after
HP–LT [47]. The type of PE used in the pouch evaluated by
Moueffak et al. [47] was not reported. The pouch tested by
Caner et al. [7] was composed of LDPE. It is possible that
different types of PE composing each pouch and processing
conditions could have caused a different seal performance
after HP–LT. In fact, LDPE is commonly used in HP–LT
applications [37]. The PET/Al/PP (CPP) films showed good
oxygen and water permeability after HP–LT. In addition,
while PET/Al/CPP [41] retained both oxygen and water
permeability, PET/Al/PP, evaluated by Mertens and
Deplace [44], had a significant reduction (greater than 25%)
in oxygen permeability. Al-based packages that maintained
visual integrity after HP–LT also showed retention of
strength properties.
No visual integrity information or oxygen permeability
has been given for other reported PE-based, PET-based,
and PP-based materials. Some exceptions included the
KOP/CPP bilayer [41], which retained both visual integ-
rity and oxygen permeability after a 600 MPa and 20 °C
treatment, and the cast oriented BOPP with a total loss
in sealability [10]. Water permeability was retained in
some of these packages; values for the PET-based pack-
age were not reported [15]. Furthermore, tensile strength
was retained in all reported materials after HP–LT.
However, the PE-based materials and CPP [10] showed a
significant (unacceptable, greater than 25%) loss in seal
strength.
Alternative reported compositions listed as ‘‘Others’’ in
Table 6 also lack information on visual integrity after HP–
LT. These materials showed acceptable water permeability
(less than 12% deviation) and, while not reported for other
materials, acceptable oxygen permeability was reported
for the BOPP/PVOH/PE laminate. These materials also
showed acceptable (less than 25% deviation) tensile
strength and elongation after HP–LT. Seal strength,
reported in only a few cases, showed significant deviation
for the Surlyn 1605 an ionomer material [10].
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Food Eng Rev (2010) 2:274–297
Overall Packaging Integrity After HP–HT
Very few studies have reported the integrity and barrier
properties of individual and multilayered composite films
after preheating and HP–HT processing (Table 7), in con-
trast to the extensive number of materials evaluated for
integrity after HP–LT processing (Table 6). Some single-
layer materials are used in the food industry, for example,
as water vapor transfer barriers. However, only a few have
been reported to survive HP–HT application, namely, PA,
EVOH, PET, PP, aluminum oxide coating [30]. In general,
all authors evaluating overall integrity after HP–HT have
reported results on visual integrity and oxygen permeabil-
ity. However, little has been reported in terms of water
permeability and strength properties; some authors only
reported the seal strength (Table 7).
Some EVOH-based materials (Table 7) were reported
to retain visual integrity after HP–HT. White stains, due to
partial delamination, have been seen in the coextruded
PA/PP/EVOH/PP after HP–HT [47]. Of all EVOH-based
materials, only the original value of the PA/EVOH pouch
met the specifications of 0.06 mL/m2/day for US military
shelf-stable products [35], or requirements for commercial
products, a specification not met after HP–HT processing.
However, where reported, oxygen permeability showed
little variation (less than 12%) after HP–HT, except for
very high increase seen in the biaxial PA/coextruded
EVOH [30] and the decrease seen in the PE/PA(Nylon6)/
EVOH/PE laminate [18]. Even though the relative
increase for the PA/EVOH laminate was very high, its
oxygen permeability after HP–HT (2 mL/m2/day) was
similar to the values reported for other HP–HT-treated
EVOH-based multilayer laminates (Table 7). Conversely,
the PA/EVOH laminate retained its seal strength after
HP–HT [30].
The only PA-based material tested at HP–HT condi-
tions, PE/PA/PE (treated at 550 MPa and 85 °C), retained
visual integrity. However, the oxygen permeability, ini-
tially greater than 0.06 mL/m2/day, was increased even
more by HP–HT. Bilaminate pouches, PA/PP and PET/PE
(Table 7), have shown visual integrity after HP–HT, except
for some blistering observed in the PA/PP [30]. Variations
of PA-based pouches in oxygen permeability after HP–HT
were significant (greater than 12%). Furthermore, none of
these materials originally met the requirements of HP–HT
for production of commercial shelf-stable products
(Table 7).
Aluminum-based pouches have shown effects from
complete delamination to minor blistering as a result of
HP–HT. Only PA/Al/PP, PET/Al/CPP, and PET/AlOx/CPP
retained integrity to a certain degree (Table 7). Neverthe-
less, materials with similar composition but from different
manufacturers provided different visual integrity after
Food Eng Rev (2010) 2:274–297
HP–HT. Although PA/Al/PP [30] showed small blisters
[56], there was observed delamination of the PE/PA/Al/PP.
Delamination of the latter was at an initial temperature of
90 °C and pressures greater than 200 MPa (between the Al
and PP layers). This difference between similar materials
could be assigned to the change in the manufacturing
process of the meals ready to eat (MRE) pouches. Fur-
thermore, PET/Al/CPP from two different manufacturers
nearly retained visual integrity after HP–HT [30], while
PET/Al/PE [47] resulted in seal breakage. It is possible that
delamination between the Al and PE layers could have
occurred in the latter material, thereby affecting seal
integrity.
Significant deviations (much greater than 12%) have
been observed in the oxygen permeability of Al-based
pouches after HP–HT [30]. All pouches originally met the
US military specifications of 0.06 mL/m2/day for shelf-
stable products [35]. PA/Al/PP and PET/Al/CPP (Smurfit
Stone) resulted in a final value of 0.4 mL/m2/day,
whereas PET/AlOx/CPP (Toppan) showed a substantial
oxygen barrier loss up to 19.6 mL/m2/day. The differences
between PET/Al/CPP pouches from two different manu-
facturers indicate the influence of the pouch-manufacturing
process on the oxygen permeability after HP–HT.
Incidence of Preheating on Packaging Integrity
After HP–HT
It has been shown that the integrity of some tested pack-
ages in terms of oxygen permeability was lost during the
preheating step up to 90 °C within 10 min [30]. Of the five
packaging materials tested (PA/coextruded EVOH, PA/PP,
PET/Al/CPP from two suppliers, and PA/Al/PP), initially
meeting the oxygen barrier criterion (0.06 mL/m2/day) for
shelf-stable products [35], none could survive the pre-
heating stage, with an increase in oxygen permeability
between 380 and 37,000% observed. Except for PA/PP, no
substantial increase (5–83%) was seen in the oxygen per-
meability of preheated packages after HP–HT.
Koutchma et al. [30] also demonstrated the influence of
preheating and subsequent HP–HT processing on seal
strength of the EVOH-based and the two Al-based mate-
rials from different suppliers. The most important effect of
HP–HT treatment coupled with preheating was found to be
the increasing seal strength of Al-based pouches (might be
due to a change in the PP layer), but the HP–HT process
did not significantly contribute to the changes in seal
strength of the EVOH-based pouch. One of the Al-based
pouches decreased in seal strength after preheating and
later on increased after HP–HT to a larger value than the
control. In addition, the fact that PP was used as the
internal layer in the Al-based pouches possibly helped to
291
provide higher seal strength in comparison with EVOH-
based pouches using EVOH as the internal layer.
Other Findings Regarding Packaging Integrity
After HPP Processing
Limited information has been reported in terms of influ-
ence of other variables after HPP on packaging integrity
and migration properties. These variables include the
headspace volume, the film thickness, the type of food
simulant contained, and the depressurization rate.
It was found that HPP induces delamination in flexible
packages made of composite materials that have a relative
large headspace volume [14, 48, 56]. Packages of PA/PE
(30 lm/60 lm) filled with CO2 showed partial delamina-
tion by bubble formation and partial loss of transparency
after 500 MPa and 300 s [16]. However, no significant
differences in seal strength of PP and two Al-based pack-
ages, sealed at low and high vacuum levels, were found
after HP–HT [30]. Nevertheless, headspace volume must
be rigorously controlled in order to minimize delamination,
flex-cracking, deformation, and stresses to the packages.
It has been questioned whether the thickness of the
packaging material might produce changes in certain
properties after HPP [10]. Some authors have not observed
changes due to the thickness of tested packaging materials
after HPP in tensile, seal strength, or global migration [33].
Information reported until now on the use of food sim-
ulants (distilled water; 15% ethyl alcohol; 3% acetic acid;
isooctane/olive oil) in a number of packages [15, 34] did
not show specific changes between simulants after HP–LT.
In a comparative study of four packages (PE/EVOH/PE,
PETmet/PE, PET/PE, and PP/SiOx) containing either
water, olive oil or sealed empty, the EVOH-based package
was the only one that showed a decrease in the melting
point when filled with water.
Little has been reported on the effect of pressurization
and depressurization after HPP on packaging integrity. Six
packages (NOD 259 (PA-PE), BB4L (internal PE), PET/
biaxially oriented polyamide (BOA)/PE, PET/PVDC/PE,
PA/surlyn, LDPE, and EVA/PE were evaluated at 10 °C
for 10 min at 200, 400 and 600 MPa, with rapid and slow
depressurization rates [37]. Permeability to water vapor
and other mechanical properties (maximal stress, tensile,
and percentage of elongation) showed no significant vari-
ations between depressurization rates at all tested pres-
sures. This data is supported by Fradin et al. [14] who
found no difference in percentage of pierced packages
due to high (1,200 MPa/min) and low (200 MPa/min)
depressurization thawing rates (200 MPa, 45 min, 25 °C).
However, an extremely fast decompression rate (20,850
MPa/min) formed white opaque areas and lines on the
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292
surface of a PP/PEF film, especially when using increased
headspace [12].
Migration and Sorption of Packaging and Food
Components
In addition to gas permeability and mechanical properties,
the integrity of packaging materials can be characterized by
sorption and migration parameters. Substances migrating
from the packaging can affect the sensory quality and level
of toxicity of the packaged product. Specifically, the food
and the packaging interact through mass transport mecha-
nisms such as permeation, sorption, and migration [6].
Volatiles, additives, monomers, and oligomers can migrate
from packaging materials into food. Likewise, volatile
compounds from the food can be adsorbed by the polymer
[57].
Global Migration
Global migration is determined by quantifying those
packaging material substances that migrate to food simu-
lants contained in the package after exposure for a period
of time. It can also be used to describe the integrity of the
package. The standard method for global migration is to
measures the amount of packaging material substance
migrated after 10 days at 40 °C in mg/dm2 from the
material surface area (AFNOR XP ENV1186-1). Under the
EU directive 90/128, plastic materials that enter into con-
tact with foodstuffs should not transfer their components in
quantities over 10 mg/dm2 from surface to the food (global
migration limit) [10].
Lambert et al. [34] tested the global migration of five
PA/PE type packages and one PET/PVDC/PE laminate
keeping packages sealed with food simulants (water, 3%
acetic acid, and 15% ethanol or isooctane) for 10 days at
40 °C. HP–LT treatment (500 MPa for 30 min at 20 °C)
did not increase the global migration, and all packages met
the referred standard (\10 mg/dm2). Similar results were
found with LLDPE/EVA/EVOH/EVA/LLDPE and PET/
Al/PP packages using olive oil as the simulant [44] and in
other packages (not reported) tested in four simulants
(water, ethyl alcohol, acetic acid, and N-heptane) [48] after
HP–LT (400 MPa, 30 min, 60 °C). Dobias et al. [10]
analyzed the global migration into 95% ethanol and iso-
octane for seven single-layer films (3 PP-based, 2 PE-
based, and 2 ethylene copolymers) and seven laminated
films (3 EVOH-based and 4 PA/PE-based). Although glo-
bal migration changed in different ways after HP–LT
(600 MPa/20 °C/60 min), even within the same types of
composition-based materials, all materials complied with
the EU directive (less than 10 mg/dm2).
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Food Eng Rev (2010) 2:274–297
Sorption of Pressurizing Medium or Food Simulant
into the Package Layers
Dobias et al. [10] tested sorption of food simulants olive oil
and water during HP–LT. No significant differences were
found between HP–LT treated and untreated controls for
14 packages (aforementioned). Absorption of aroma com-
pounds such as acetophenone and p-cymene were studied
in PET/Al/LDPE and two PE-based packages at 500 MPa
and 25 °C for up to 60 h [32]. While p-cymene was less
absorbed by HP–LT-treated packages than by the untreated
packages, acetophenone was not absorbed by the Al-based
package at both atmospheric and HP–LT conditions. Due
to the absorption observed in controls at atmospheric
pressure, it may be possible that more p-cymene is absor-
bed by the HP–LT-treated package during storage.
A study on individual packages showed that LDPE,
CPP, EVA, PET are more prone to absorb d-limonene than
EVOH, PVOH, and PVDC both before and after HP–LT
(400 MPa at 20 °C for 30 min) [41].
Diffusion of Compounds into or Out of Packages
After HPP
The kinetics of diffusion of acetophenone and p-cymene
through PET/Al/LDPE and two PE-based packages [32]
was evaluated at various holding times up to 60 h at
500 MPa and room temperature. Pressure significantly
decreased the diffusion of both substances in PE-based
packages, while the Al-based package remained imper-
meable to either substance at all pressure levels. Imper-
meability of the PET/Al/LDPE to p-cymene package
(50 MPa/25 min, 23 °C) was verified by other authors
[16]. The decrease in migration rate might be attributed to
an increase in the glass transition temperature of the
package due to pressurization, according to Kubel’s
hypothesis [32]. However, it has also been argued that the
structural damage (delamination, detachment, cracks, and
folds) observed during pressurization can substantially
increase diffusion rate.
A study [56] on the migration of components in the
pressurizing liquids into the package confirmed the
impermeability of the aluminum layer in a retort package
(PE/PA/Al/PP). Aluminum layer was impermeable to the
migration of 1,2-propanediol contained in the pressurizing
fluid into the package containing 95% ethanol at both
HP–LT (400–827 MPa and 30–50 °C) and HP–HT
(600–827 MPa and 75 °C) for 10 min. However, an
EVOH-based package (PA/EVOH/PE) showed significant
migration of 1,2-propanediol. In this case, pressures higher
than 200 MPa significantly reduced migration levels
compared to non-pressure-treated packages.
Food Eng Rev (2010) 2:274–297
Other Testing Approaches for Evaluation of HPP
Effects on Packaging Materials
Microscopy
Scanning electron microscopy (SEM) has been applied to
detect damages (e.g., delamination, detachment, crack, and
folds) to the external surfaces of packages after HPP
treatment [8, 15, 16]. For example, SEM demonstrated an
increase in tensile strength of a silicon-based material
(PP/SiOx) after 400 MPa and 60 °C, showing that the
structure is completely broken after HPP. Delamination,
detachment, cracks and folds are indirectly associated with
increased permeation rates of aroma compounds such a
p-cymene [16]. By means of SEM, Caner et al. [8] iden-
tified small wrinkles in packaging materials PET/Al2O3/
LDPE, PET/SiOx/LDPE and PET/PVDC/4%EVA/LLDPE
after HPP (800 MPa and 45 °C), showing that physical
integrity was not affected. However, numerous fold and
wrinkles were seen on the food contact layer of a MET–
PET material, making it not suitable for HPP.
Even though SEM shows damage in superficial layers, it
is not directly associated with damage to barrier layers such
as Al2O3 and SiOx. Changes in these thin barrier layers are
not detectable through mechanical testing even though
permeability could change. Scanning acoustic microscopy
(C-SAM) has been utilized as an alternative to provide
subsurface information on various plastics. C-SAM can
detect, classify, and accurately produce an image of opaque
materials using ultrasonic waves ranging from 5 to
500 MHz by means of a pulsed focused beam in a raster
pattern over a sample [8]. This technique can show changes
in elastic properties occurring between two constituents in
a multilayer structure or within one constituent. Air pockets
and gaps constituting the sublayers as small as 10-7 can be
detected, as well as cracks, folds, delamination, and
porosity of solid samples.
For example, in the case of the MET-PET film [8],
C-SAM confirmed that delamination occurred between the
food contact PET layer and aluminum layer at random
locations, increasing with pressure holding time.
Differential Scanning Calorimetry
Differential scanning calorimetry (DSC) can be used to
investigate the ability of HPP to cause changes in the
melting point and crystallinity of several materials. The
analysis requires a calorimeter that scans a small piece of
sample at near room temperature, up to a very high tem-
perature (aprox. 300 °C), at specified heating and cooling
rates (generally 10 °C/min) in a small piece of sample.
Standards have been developed to determine melting and
crystallization temperatures [2]. Melting temperatures are
293
determined from the maximum of the endotherm and
enthalpies of fusion, calculated by integrating the respec-
tive melting endotherm.
Little has been studied on package crystallinity after
HPP [15, 39, 56]. Schauwecker et al. [56] found no changes
in melting point or percentage of crystallinity after
600 MPa and 95 °C in PA/EVOH/PE and PE/PA/Al/PP
pouches. Lopez-Rubio et al. [39] also measured the melting
point as well as the enthalpy of fusion in two EVOH-based
pouches (Table 7) after 800 MPa and 75 °C, finding no
difference in melting point for the EVOH26 and EVOH48
compared to the untreated control. However, higher melt-
ing enthalpies after HPP indicated a pressure-induced
crystallinity development, not seen by Schauwecker et al.
[56]. On the other hand, results from Galotto et al. [15]
are not in accordance with other authors [39, 56], since
a decrease in both melting point and enthalpy in
PE/EVOH/PE (containing either olive oil or aqueous sim-
ulant) after 400 MPa and 20 °C/60 °C was found (attrib-
uted to lower crystal size and less crystallinity). In contrast,
Galotto et al. [15] found no changes in melting point nor
enthalpy in the materials PET/PE or PETmet/PE at
400 MPa and 60 °C.
Fourier Transform Infrared Spectroscopy
Fourier transform infrared spectroscopy (FT-IR) transmis-
sion experiments were used to determine detect crystal-
linity alterations through molecular changes in EVOH and
retort packages [39, 56]. The aim was to observe changes
in infrared bands associated with crystallinity, which were
assigned to C–O–C stretching or C–C stretching, as well as
changes in humidity through observation of the OH band.
Even though [56] found equivalent absorbance bands of
EVOH-based and PE/PA/Al/PP tested films before and
after pressure, Lopez-Rubio et al. [39] found an increased
absorbance in the crystallinity band (1,140 cm-1) of the
HPP-treated EVOH26 material. This indicated a higher
crystallinity in EVOH26 material after pressure. A change
in crystallinity or molecular structure by means of FT-IR
was not observed for the EVOH48 after HPP. Proper
comparison of all packages utilizing the same conditions
will provide a better explanation on thermal behavior,
including the comparisons in the presence of water and at
dry state.
X-Ray Diffraction
X-ray diffraction is a fingerprinting technique designed to
determine the degree of crystallinity of a polymer. This
technique measures the level of diffraction caused by the
material after radiation with an X-ray source. Lopez-Rubio
et al. [39] found minor changes with X-ray diffractograms
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294
in EVOH26 and EVOH48 materials although EVOH26
showed shifts toward higher angles and narrower peaks,
which also contributed to support findings in increase of
crystallinity structure using FT-IR.
Final Remarks
This review has defined the integrity criteria to be met by a
packaging material after HPP processing at mild and high
temperature (i.e., visual integrity, gas permeability, seal
and physical strength properties, and global migration of
packaging components into the food; Table 3). At least one
of these properties was not assessed for packages reported
in each study reviewed, not enabling a complete screening
of packaging after HPP. In addition, there is variation in
HPP conditions reported due to differences in maximum
pressure and temperature achievable by laboratory HPP
units. These conditions can also provide different outputs
in terms of decontamination or sterilization efficiency.
Among all integrity properties, failure in visual integrity by
delamination or blistering suffices to discard the material
for a given processing condition. In addition, specific tol-
erances have been defined for HP–HT and retort in terms of
gas permeability for shelf-stable products. However, apart
from a percentage of deviations defined by industrial
norms, specific tolerances need to be defined for strength
properties as well as gas permeability at HP–LT conditions.
Evaluations on visual integrity, gas permeability, seal
and physical strength properties of packaging materials
treated at HP–LT conditions are commonly found in the
literature. These properties have been tabulated for
screening reported packages arranged according to their
main gas barrier (i.e., EVOH, PVDC, PA, SiOx, Al/metal-
ized, etc.) with the aim of determining deviations after HP–
LT according to European or Japanese standards (Tables 3
and 4). Not all the materials, however, have been evaluated
for integrity after HP-LT. Even though changes in oxygen
and water permeability are reported, this may not indicate
that certain packages do not meet barrier requirements for
certain refrigerated product applications. For example,
some PVDC-based and PA-based materials exceeded gas
permeability by more than the standard 12% after HP–LT
but still remained within initial values reported for similar
types of materials tested by other authors (Table 6). The
same was observed for strength properties like tensile
strength in materials exceeding the standard 25% deviation
limit (e.g., PVDC-based and PA-based materials).
In general, reported EVOH-based materials showed
no deviations after HP–LT in terms of visual integrity,
permeability, and physical properties. Nevertheless, infor-
mation gaps for certain properties, including global
migration, must be provided for a complete assessment of
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Food Eng Rev (2010) 2:274–297
the suitability of some reported materials. Even though,
PA-based laminates showed lower gas barrier properties
than EVOH, a common trend was the increase in tensile
strength after HP–LT. Some metalized materials showed
delamination after HP–LT and their visual integrity and
seal properties depended on the external layers used by the
laminates (PP or PE) and possibly the type of adhesives
used between layers [34]. Those metalized materials that
retained visual integrity seemed to also retain oxygen and
water permeability and strength properties. Further testing
is required to assess KOP-based materials and other PE-,
PET-, PP-based materials not combined with high oxygen
barriers such as EVOH, PVDC, PA or Al.
One of the most important outcomes in the search for
pouches suitable for HP–HT conditions is that the pre-
heating process can affect the overall integrity of the
package, especially when temperatures around 90 °C are
used. For packaging materials surviving the preheating
process in terms of visual integrity, oxygen permeability
changes observed between preheating and HP–HT were
minor [30]. Most results reported in the literature for
packages treated at HP–HT conditions mainly reported on
visual integrity and oxygen permeability. However, further
testing is needed to complete an overall integrity assess-
ment after HP–HT according to the requirements defined
before in Table 3.
Some EVOH materials, a PA-based material, and a few
Al-based/metalized pouches showed acceptable visual
integrity after HP–HT. The variations in oxygen perme-
ability of EVOH-based pouches and the PA-based pouch
remained within the standard 12% after HP–HT; however,
Al-based/metalized pouches (acceptable in visual integrity)
had much larger variations after HP–HT. The oxygen
permeability value requirement for shelf-stable products
(0.06 mL/m2/day for the US Army and 0.2 mL/m2/day for
some commercial products) was not met by most tested
materials even without processing nor was it met by all
materials after HP–HT. However, the oxygen barrier tol-
erance specified for shelf-stable MREs is relative and
highly dependent on the food type being processed. Other
authors have found materials currently used for retort
processing (Al-based/metalized or EVOH-based) that pro-
vided adequate protection with oxygen transmission values
greater than 0.5 mL/m2/day after retorting [18, 30]. Fur-
thermore, it has been reported that for some laminates the
permeability values vary during storage and at different
relative humidity [58]. Thus, the significance in terms of
changes in oxygen permeability after HP–HT should be
revisited and defined according to specific product appli-
cations. Further exploration is required for PVDC and SiOx
laminates after HP–HT.
The residual headspace in certain packages has
been shown to influence package integrity by causing
Food Eng Rev (2010) 2:274–297
delamination. Thus, headspace must be minimized not only
to maximize vessel use capacity but also to maintain
integrity. Further work must be done in order to establish a
minimum headspace value acceptable to maintain package
integrity at both HP–LT and HP–HT conditions.
Little work has been done on global migration, package
sorption and substance diffusion in HP-treated packages.
Some packages have been found to comply with the
AFNOR norm (\10 mg/dm2) for global migration after
HP–LT. Further global migration studies are required to
determine if packaging components are released into the
food after HP–HT treatments. The global migration of the
packages may or may not be correlated with the thickness
of the film, the nature of the materials, or the fabrication
process. Furthermore, packages do not absorb excess liq-
uids such as water or olive oil into the structure after
HP–LT. The absorption into the package structure of aroma
compounds contained in the package or in the compression
fluid has been decreased during HP–LT. However, further
work needs to be undertaken to determine if there are
sorption effects during storage after HPP. On the other
hand, HPP has been found to decrease diffusion of aroma
compounds through the package [16, 32].
Other techniques such as SEM, C-SAM, DSC, FT-IR,
and X-ray diffraction were presented to support findings on
overall integrity properties after HPP by explaining struc-
tural and physicochemical changes in tested materials.
SEM can identify material damage (delamination or
cracks) not recognized by the naked eye. This information
could help explain changes in strength or barrier properties
as a result of stress transformations at the micro level.
C-SAM can complement SEM results by providing sub-
surface information, possibly related to sorption, diffusion
or gas permeability. Changes in crystallinity and melting
point can be followed by DSC, and crystallinity results can
be supplemented by information provided from the FT-IR
and X-ray diffraction. Further research should provide
information about the changes in crystallinity that may lead
to delamination.
Further research is required in screening new materials
that are finding applications in thermal processing (hot fill
or retort) for their potential use in HPP processes [36, 58].
The identification of transparent materials is desirable due
to higher consumer preference [36]. For example, thin
vacuum deposited coatings of SiOx on PET, PP or PA,
which have been suggested to be transparent, water-resis-
tant, retortable microwaveable options, have been sug-
gested. Another option is the evaluation of new barrier
polymers currently used as discrete layers with an oxygen
permeability value 50–100 times lower than PET. Fur-
thermore, biodegradable polymers such as 3-hydroxy
butyrate co 3-hydroxy hexanoate (PHBH) are being
developed with oxygen barrier properties resembling those
295
of EVOH, with heat sealability and resistance to grease. In
addition, blends of barrier polymers and standard polymers
have been developed, including EVOH in PP, PE or PA;
PA in PP or PET, and LCP in PET and PE [36]. Last but
not least, other nanocomposite materials, or polymers filled
with small (100–1,000 nm) inorganic particles, may
improve barrier properties by a factor of 50 or higher.
There is a trend to use more plastic-based, stronger,
packaging materials that provide higher durability and
meet the demand for higher line speeds and packaging
waste reduction. Other newer barrier technologies which
have been appearing are providing innovations that may be
suitable for HPP.
A few materials utilizing PET, PE, PP, as well as
PS-EVOH, PE-EVOH, and other metallic films are cur-
rently being utilized for commercial production. Even
though the data provided by the scientific literature does
not provide all the specifications required to determine
their suitability for HP–LT applications, available infor-
mation indicates positive results for some of these material
combinations. In the case of packaging for HP–HT EVOH-
based materials show potential for this application since, in
some cases, visual integrity and oxygen permeability were
retained. Due to the increased commercialization of high-
pressure products and the appearance of industrial units in
the last decade, standardized studies carried out at com-
mercial processing conditions would allow a better
understanding of what types of packaging material barriers
can better suit HPP. Once all requirements for HP–LT and
HP–HT packages have been thoroughly defined by the
industry for specific product applications, more complete
studies on materials will provide the whole picture that can
assess their suitability for HP process.
Acknowledgments The authors are very grateful for the informa-
tion provided by Dr. Carole Tonello at NC Hyperbaric. We would
also like to thank Mr. Michael Kelly from CSIRO for his contribution
as CSIRO internal reviewer.
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