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Packaging and the Shelf Life of Coffee

Lara Manzocco, Sofia Melchior, Sonia Calligaris, and Maria Cristina Nicoli, Department of Agricultural, Food, Environmental and
Animal Sciences, University of Udine, Udine, Italy
© 2019 Elsevier Inc. All rights reserved.

Introduction 1
Roasted Coffee 1
Quality Depletion of Roasted Coffee During Storage 3
Packaging of Roasted Coffee 3
Instant Coffee, Coffee Concentrates and Coffee Beverages 6
Instant Coffee 6
Quality Loss of Instant Coffee During Storage 7
Packaging of Instant Coffee 7
Coffee Concentrates and Beverages 8
Quality Loss of Coffee Concentrates and Beverages During Storage 8
Packaging of Coffee Concentrates and Beverages 8
Shelf Life Assessment of Coffee Products 8
Consideration on the Secondary Shelf Life of Coffee Products 12
Conclusions 13
References 13

Introduction

The food industry is currently confronted with the major challenge of providing affordable, nutritious, and safe food to a continu-
ously growing population. The traditional paradigm based on the increase of food production is no more sustainable, nor econom-
ically feasible. A strategic trend is to ensure food supply by optimizing the use of resources while minimizing the risk for food waste.
The latter often occurs during the distribution and consumption stages of the food chain and can be tackled by improving the
management of food shelf life. In this context, the two strongest driving forces are: (i) the choice of packaging materials/processes
fitting with the stringent requirements of performance and sustainability; (ii) the optimal management of the quality of the prod-
ucts on the market, based on accurate estimates of food shelf-life. In the case of coffee products, due to the wide number of dete-
riorative mechanisms that could affect their quality decay, these are complex tasks and should be carefully designed depending on
the product peculiarities. From one side, rigorous matching of product protection needs and packaging protective performance
should be performed. From the other side, systematic planning of shelf life assessment and validation should aim at quickly
producing shelf life data really accounting for consumer behavior.
This article first discusses the main classes of coffee products available on the market (roasted whole and ground coffee, instant
coffee, coffee concentrates and beverages) focusing on processing technologies, events responsible for their quality decay, and pack-
aging strategies. Then the basic steps of shelf life assessment protocols of coffee products are described together with some examples.

Roasted Coffee

Coffee is one of the most popular beverages all over the world, with a global forecast consumption of 167.9 bags in 2019/2020,
which correspond to 2 billion cups consumed every day (USDA Foreign Agricultural Service, 2019).
Coffee is prepared from roasted beans of several species of the genus Coffea, although two main species are generally used for
commercial production: Coffea arabica, which accounts for approximately 70% of the global coffee market, and Coffee canephora,
also known as Robusta coffee. These two species differ in terms of optimal growing conditions, composition and brew character-
istics. Robusta coffee, for example, is characterized by less desirable flavor while Arabica has a delightful aroma and superior quality
(Cannon et al., 2010; Farah, 2012). The process that turns green coffee beans into roasted coffee involves the series of steps reported
in Fig. 1.
After arrival and sorting, green coffee beans, are submitted to the roasting process. It should be noted that, before roasting, green
coffee beans can be submitted to a decaffeination process to obtain remove caffeine by solvent extraction, water extraction or super-
critical carbon dioxide extraction (Katz, 1987; Heilman, 2001; Lisboa et al., 2019).

Reference Module in Food Sciences https://doi.org/10.1016/B978-0-08-100596-5.22656-5 1


2 Packaging and the Shelf Life of Coffee

Figure 1 Key technological steps to obtain whole roasted coffee beans and ground roasted coffee.

Roasting is the main unit operation in the coffee industry. It can be defined as an intense heat treatment (T > 200  C) which
completely changes color, flavor and taste of green beans (Clarke, 1987a). These changes are due to several chemical, physical
and structural modifications occurring as a consequence of the temperature increase in the roaster, where hot gases or metallic
surfaces are in contact with coffee beans. The process is usually characterized by the following consecutive stages, according to
the temperature of the beans.
- Temperature increase from ambient to about 150  C
The temperature of the beans increases progressively until reaching the evaporation temperature of the bean water. Initially, the
generated vapor cannot permeate and pressure built-up makes bean volume expand. When the pressure is high enough, the shell
of the bean snaps. During this phase, bean color changes from green to yellow, and aroma starts to develop mainly due to the devel-
opment of the early steps of Maillard reaction in concomitance with isomerization and lactonization of chlorogenic acids
(Fernandes, 2019).
- Temperature from 150 to 180  C
Color changes from light yellow to brown due to non-enzymatic browning reaction development. Roasting reactions move towards
the inner dry structure of the bean. Beans become brittle and some little fissures at the surface occur. Aroma formation starts. Sugars,
especially sucrose, caramelize and acidity increases due to the formation of carboxylic acids from carbohydrates degradation.
- Temperature from 180 to 230  C or more
Coffee bean color gets darker and darker while expanding due to the high inner pressure caused by water vapor, CO2 and volatile
compounds, formed as a consequence of the Maillard reaction. Upon their release, weight loss and rupture of bean internal structure
are observed. Furthermore, pyrolysis and caramelization take place. The latter causes the development of sweetness and pleasant
flavors. Acidity also drops due to acid degradation.
- Temperature decrease
To stop the roasting process and avoid roasted coffee burning, hot beans are submitted to cooling by water quenching or air, until
room temperature is reached (Eggers and Pietsch, 2001).
It is clear that, during this complex process, the physical and chemical composition of the coffee beans is strongly modified.
Hundreds of different volatile and non-volatile compounds are formed, being responsible for the sensory profile of coffee. Among
non-volatile compounds, melanoidins are responsible for the typical dark color. In addition, these molecules, especially those of
low-molecular weight, act both as primary and secondary antioxidants (Moreira et al., 2012). A strong antioxidant activity is also
exerted by phenolic acids such as chlorogenic and coumaric, caffeic and ferulic as well as heat-induced polyphenol-like structures
which are formed during non-enzymatic browning reactions (Anese and Nicoli, 2003; Cheong et al., 2013; Yashin et al., 2013).
Besides these beneficial compounds, other molecules formed during the Maillard reaction can be toxic, mutagenic or carcinogenic
to the human body. Two examples are 5-hydroxymethylfurfural (HMF) and acrylamide. The latter was added to the list of food
borne toxicants in 2002 and coffee appears to be one of the major contributors to the overall intake. Acrylamide is formed at
the beginning of roasting and within 2 minutes its level rapidly drops. This behavior can be attributed to reactions or
Packaging and the Shelf Life of Coffee 3

polymerization of this compound with other coffee components upon further roasting. For this reason, the more intense the roast-
ing, the lower its acrylamide content (Anese et al., 2013; Claeys et al., 2005; Michalak et al., 2016).
The formation of volatiles and CO2 causes bean expansion and rupture of its internal structure due to the high pressure gener-
ated. As a consequence, beans become brittle, porous and unable to entrap volatiles which are easily released during storage. After
roasting, coffee is rich in gases, mainly CO2 (87%), but also carbon monoxide (7.3%) and nitrogen (5.3%). The rest (1%) is rep-
resented by volatile organic compounds (Clark, 1987a; Wang and Lim, 2017). The massive degassing that takes place in the first
hours after roasting slows down gradually. This phase requires 360 h and up to 2400 h for roasted and roasted whole coffee, respec-
tively. The process is slow because CO2 is bound to the bean structure. Nevertheless, it was reported that during degassing, shelf life
is reduced by 10% for every 24 h at room temperature in air (Anderson et al., 2003; Wang and Lim, 2014). In addition, CO2 acts as
a barrier, reducing the contact between oil and air. Upon CO2 release, oil is forced from the inner part of the matrix to the surface,
where the oxidation risk is higher. Oil exudation could cause particle stickiness and aggregation, which finally leads to irregular
brewing (Nicoli and Savonitti, 2005; Wang and Lim, 2014; Yeretzian et al., 2017).
It should be noted that the degassing phase can be skipped to preserve aromas and flavors. However, in this case, proper pack-
aging solutions should be implemented to avoid package swelling during storage (e.g. use of one-way safety valve discussed later).
Whole roasted coffee beans are sold after proper packaging or can be subjected to grinding. This treatment is needed to increase
the specific surface area and promote the transfer of soluble and emulsifiable substances from the coffee matrix to water during
brewing (Farah, 2012; Petracco, 2005). After grinding, coffee is packaged to meet market demand for product protection and
stability. Whether roasted coffee is marketed as whole or ground product, the selection of the most appropriate packaging solution
requires understanding of the mechanisms of the possible deteriorative reactions affecting its quality and shelf life.

Quality Depletion of Roasted Coffee During Storage


After roasting, the huge number of newly-formed compounds as well as those naturally present readily undergo further chemical
reactions. Oxidation is certainly among the most important phenomena in roasted coffee. As is well known, oxidation in foods is
a complex set of reactions, involving firstly molecules belonging to the lipid family and oxygen, and leading to the formation of
a number of radical and highly reactive species. The lipid fraction of coffee accounts for about 11%–17% (w/w) and is rich in unsat-
urated fatty acids, especially linoleic acid which is particularly prone to oxidation (Toci et al., 2013; Toledo et al., 2016; Vila et al.,
2005). When lipid oxidation takes place during storage, it causes the formation of undesirable flavors, making the product less
acceptable, or totally unacceptable to consumers, and determining the end of its shelf life.
Beside oxidation, the flavor profile could also change due to volatile release. For instance, thiols are coffee-odorants whose vola-
tilization is in general associated with a decrease in the coffee sensory quality (Dulsat-Serra et al., 2016). Thus, just after roasting,
coffee starts to lose flavors, progressively reducing its quality characteristics. The concomitant development of oxidative reactions
and flavor loss is responsible for the so-called coffee staling, which is defined as “a sweet but unpleasant flavor and aroma of roasted
coffee which reflects the oxidation of many of the pleasant volatiles and the loss of others; a change in the flavor and the acid constit-
uents causing a partial bland tone” (Sivetz, 1963). The kinetics of staling mainly depend on the environmental conditions suffered
by coffee beans after roasting. For instance, the increase in storage temperature might favor both volatile release and oxidative reac-
tions, while the latter are accelerated by light exposure and oxygen concentrations in the headspace. In addition, the role of water
vapor in the headspace should not be neglected. At moisture contents above that of the monolayer, water would compete for the
polar sites of the coffee matrix, disrupting the interactions among carbohydrates which physically entrap the volatiles. The final
result is thus an intense volatile loss, which is particularly important for polar volatile compounds (Flink and Karel, 1972).
Due to this complexity, monitoring staling during roasting is not an easy task. Different indices have been proposed in the liter-
ature; some of them are associated with the development of oxidation (e.g. hexanal), others to flavor loss (e.g. thiols) or to the
formation and degradation of selected compounds. The list of these indicators is presented in Table 1. Moreover, the ratio between
unsaturated and saturated fatty acids from both free fatty acids and triacylglycerols has been investigated, resulting in a potential
tool to monitor roasted coffee oxidation during storage (Toci et al., 2013). Sensory analysis by sniffing coffee powders or tasting
coffee brews has also been widely adopted to monitor the evolution of staling during coffee storage. It should be noted that micro-
bial growth is never an issue in whole and ground roasted coffee. The low water activity of coffee, together with the lack of essential
nutrients and the peculiar content of melanoidins with antimicrobial properties, prevent microbial spoilage.
Beside coffee staling, moisture adsorption should be not underestimated. For this reason, sorption isotherms data could be
useful to predict optimum storage and trading conditions to ensure quality (De Oliveira et al., 2017).

Packaging of Roasted Coffee


The choice of coffee packaging material and technology is fundamental in order to reduce the rate of staling and ensure the longest
possible shelf life of roasted coffee products. The package should meet specific quality requirements. It has to act as a barrier against
environmental stresses (water, atmospheric oxygen, light), while being greaseproof to avoid mechanical damage upon absorption
of oil from the coffee bean surface. In addition, the material should be cheap and with high convenience (easy-to-open; resealable,
environmentally-friendly). It should also comply with any relevant regulations regarding the limits for contaminant migration from
the packaging to the product. This is certainly an important issue since contact time between packaging and coffee product is
4 Packaging and the Shelf Life of Coffee

Table 1 Possible indices of staling during storage of roasted coffee

Indices Reference

M/M aroma index (methanol/2-methylfuran) Vitzhum and Werkhoff


(1978)
2-butanone/2-methylfuran Glöss et al. (2014)
2,3-butanedione/2-methylfuran Glöss et al., (2014)
Dimethyl disulfide/methanethiol Glöss et al., 2014
2-furfurylthiol/hexanal Marin et al. (2008)
2-butanone/methanethiol Glöss et al. (2014)
Furfural Makri et al. (2011)
Flavor quality index (based on hexanal, vinylpyrazine, pyrrol, furfuryl-methylketone and pyridine content) Spadone and Liardon (1989)
S aroma index (sum of the 2-methylpropanal, 3-methylbutanal, diacetyl and 2-methylfuran) Radtke and Piringer (1981)
Sensory attributes Kreuml et al. (2013)
Makri et al. (2011)
Rendón et al. (2014)
Ross et al. (2006)
Stokes et al. (2017)
Peroxide values Nicoli et al. (1993)
Unsaturated FA/saturated FA Toci et al. (2013)

expected to be rather long. In addition, contaminant migration could be particularly crucial when dealing with novel materials,
which are increasingly requested by the market to meet sustainability targets.
- Packaging technologies
The extension of roasted coffee quality is not just the result of the right packaging material but depends on its combination with an
adequate packaging technology, which is often applied to reduce oxygen concentration in the package. As previously described,
oxygen is the main environmental factor affecting the rate of oxidative reactions occurring inside the coffee package. Thus, its reduc-
tion from 21% (air) to less than 1% allows a significant extension of coffee product life, generally longer than 12–18 months, as
declared by the producers. Table 2 shows the most widely used packaging technologies applied for whole and ground roasted coffee
products. Vacuum packaging ensures the removal of headspace air, leading oxygen concentration to a level around 4%–6%, and can
be applied in combination with both flexible and rigid materials. In the latter, more volatilization phenomena occur due to the
saturation of the headspace caused by the difference between partial pressure of ambient and aroma compounds. A further option
is based on air substitution with inert gas (usually nitrogen) by flushing the package headspace or through compensated vacuum
technique. This technique is called modified atmosphere packaging and results in a residual oxygen concentration of about 1%–2%.
Pressurization acts in the same way, but in this case the internal pressure is higher than the atmospheric one. Only rigid materials
can be used for this purpose and they must incorporate a safety valve which will open if the pressure is too high (Nicoli and Savo-
nitti, 2005). Due to the technological procedures applied during pressurization, oxygen content is further reduced to less than 1%.
Active packaging solutions are also available. These are based on “packaging that changes the condition of packaged food to
extend shelf life or improve food safety or sensory properties, while maintaining the quality of packaged food”. These systems
include the use of absorbers (scavenging system) and emitters (active-releasing system), and usually act to reduce oxygen concen-
tration to less than 1% (Nicoli and Savonitti, 2005). They might be used in rigid cans and pods and come in different forms such as
films, sheets, sachets, coatings and granules (Lee, 2016).
- Packaging materials

Table 2 Expected oxygen content in the


headspace in contact with
coffee products by using
different packaging techniques

Oxygen
Packaging technique (%)

Air 21
Under vacuum 4–6
Inert gas 1–2
Pressurization <1
Active packaging <1

Modified from Nicoli et al. (2010).


Packaging and the Shelf Life of Coffee 5

Table 3 Main packaging materials for roasted coffee. Barrier properties against oxygen and moisture, potential recyclability and headspace
atmosphere are also reported

Package Material Head space Barrier properties Recyclability

Bag Cardboard Air Low Total


Flexible laminated aluminum with or without safety Vacuum, modified atmosphere High None
valve
Can Tinplate with or without safety valve Air, vacuum, modified atmosphere, Total Total
pressurization
Aluminum multilayered materialsþ external Air, modified atmosphere High None
cardboard
Capsules Primary: Aluminum Modified atmosphere Total None
Secondary: cardboard None Total
Primary: Plastic polymers (e.g. polypropylene) None None
Secondary: aluminum multilayered materials High None
Pods/pads Primary: Filter paper Modified atmosphere Low Total
Secondary: aluminum multi layered materials High None

Table 3 summarizes the main packaging materials used for marketing whole and ground roasted coffee, along with the packaging
techniques used to eventually modify the composition of the atmosphere in contact with the product. A general indication about
barrier properties and potential recyclability of the packaging material is also reported. Cardboard bags are the oldest type of pack-
aging used to store and sell roasted whole beans. Obviously, due to its high permeability to oxygen and water, coffee in cardboard
bags is in contact with air. This implies a high oxygen level in the bag headspace and thus a short shelf life, estimated to be around
1 month (Nicoli et al., 2010). For this reason, today, this packaging material is used to retail coffee in local markets, directly from
small roasting facilities, mainly in countries producing green coffee. However, being paper a material with a potentially high
sustainability since it is completely recyclable, and considering the evolving global market need for sustainable packaging solutions,
it is not excluded that the use of cardboard for specialty coffee will expand in the near future also in countries with high coffee
consumption.
Today the most widely diffused, cheap and easy-to-manage packaging material is polymer-aluminum multiply laminates. The
central layer is aluminum foil which is able to guarantee an efficient oxygen barrier. A water vapor barrier and mechanical strength
are then due to the inner and outer polymer layers respectively. Due to their physical characteristics, vacuum packaging as well as
modified atmosphere packaging can be used to pack both degassed or not degassed roasted coffee. In the latter case, to avoid the
swelling of the package during storage, a one-way safety valve can be incorporated in the material to allow CO2 to escape, while
keeping volatiles inside without letting oxygen and contaminants enter (Eubanks, 2009; Smrke et al., 2018).
Cans made of tinplate are also widely used for coffee packaging. Tinplate can be regarded as a total barrier material, resistant to
pressure and also recyclable, but expensive and rigid, and comes in shapes that do not allow the optimal use of space. Based on this,
all the packaging techniques previously mentioned can be adopted. Interestingly, this is the only material supporting pressurization
as a packaging technology. It can withstand pressures higher than atmospheric generated inside the container as a consequence of
coffee degassing and, for this reason, the container must be equipped with a safety valve (Nicoli and Savonitti, 2005).
Historically, roasted coffee is packed in multidose containers, allowing its parceled use for multiple coffee brew preparation at
home, bar or catering facilities. The invention of the coffee capsules and pods has revolutionized coffee drinking. Capsules and pods
are designed for specific coffee machines and contain the optimal quantity of coffee powder for a single-cup preparation. The initial
target was the preparation of espresso coffee at home, but today other types of coffee preparations, packaged in capsules or pods, are
proposed. Coffee E.S.E. (Easy serving espresso) pods are made of 7 g of roast and ground coffee, packed in two fine layers of filter
paper, which can be directly inserted in the brewing machine. These pods have only three constant diameters of 44 (widely used), 38
or 55 mm and can be universally used in machines for E.S.E. pods extraction. The advantage is that after use, the pods can be
disposed of as organic material. From the other side, being the primary package made of filter paper without barrier properties,
a secondary package is required to preserve coffee quality during storage. This is why pods are frequently sealed into a secondary
package made of combined multiply polymer aluminum and saturated with an inert gas. Similarly to coffee pods, coffee capsules
are designed for specific espresso machines but they may contain different amounts of coffee (5–7.5 g) packaged in plastic or
aluminum material, and conditioned in a modified atmosphere (Albanese et al., 2009; Nicoli et al., 2010). Also in this case
a secondary package is necessary, whose barrier level depends on the barrier level of the primary package. For instance, when coffee
is packaged in aluminum capsules, the secondary package is generally made of cardboard. Conversely, if coffee capsules do not
contain an aluminum barrier, the secondary package is often a flexible laminate or a metal can.
The standard materials used for packaging of coffee capsules/pods have raised important environmental concerns due to the
intensive use of non-renewable oil. In addition, capsules cannot be recycled at municipal facilities because they are often made
of multiple materials and need to be emptied. It has been estimated that PE, PET and aluminum downstream production, related
to coffee-capsule production, could generate more than 400,000 tons of emitted CO2. In an attempt to reduce the carbon footprint
of food packaging and increase its degradability in the environment, a novel packaging approach is represented by the use of
6 Packaging and the Shelf Life of Coffee

biobased polymers. However, even the promising polylactic acid (PLA) was demonstrated to be inadequate for coffee packaging due
to poor mechanical strength, thermal resistance and permeability. A number of different novel materials are nowadays claimed to
ensure product quality while reducing waste (Nicoli and Savonitti, 2005; Nicoli et al., 2010; Lee, 2016). However, further research is
needed to evaluate their effectiveness in food protection. For this reason, some companies are trying to compromise the opposite
needs of product protection and sustainability by replacing petroleum-derived PE packaging with biobased PE packaging.

Instant Coffee, Coffee Concentrates and Coffee Beverages

Beside whole and ground coffee products, a number of other coffee derivatives is available on the market. They mainly comprise
instant coffee products and ready-to-drink beverages. Both categories are characterized by a high convenience, considerably
reducing or nullifying the time needed for coffee preparation at home. In fact, coffee extraction is industrially performed on a large
scale before further processing (Fig. 2). Basically, a solid-liquid extraction is applied to separate water soluble solids and volatile
aroma/flavor compounds from ground roasted coffee beans. The process can be conducted at atmospheric pressure with water
at temperatures around 100  C or under pressure with water temperature around 170  C. The process is arranged, differently
from home extraction, in multi-stage (percolation batteries) or in continuous countercurrent operation to efficiently extract coffee
compounds until a concentration adequate for further processing is achieved (Clarke, 2001). The extraction yield can be managed
by modifying the time, temperature and pressure of the extraction phase. It should be noted that in many cases a volatile aroma
recovery phase is carried out before coffee extraction. Alternatively, stripping of volatile compounds can be performed along
with coffee extraction. Recovered coffee volatiles are then reincorporated into the final product to re-establish its overall flavor.
After the extraction phase, the coffee brew is generally clarified through centrifugal clarifier or filters with the aim of separating
the insoluble solids. At this point, coffee extracts are submitted to a concentration process to standardize the product characteristics
as well as reduce the amount of water removed during further drying steps. The concentration phase can be mainly performed by
applying three different types of processes: thermal concentration, cryo-concentration or membrane concentration. The choice
depends on the target quality of the final product. Coffee concentrate is the output of this phase and can be considered as
a semi-manufactured product to be further processed into instant coffee or coffee beverages (Fig. 2). It should be noted that coffee
concentrates are not only used at industrial facilities but are also packaged and sold as flavoring ingredient for different products
(e.g. ice cream and chocolate derivatives).

Instant Coffee
Instant coffee, also called soluble coffee, coffee crystals, or coffee powder, is defined as “dry product, water soluble, obtained exclu-
sively from roasted coffee by physical methods using water as the only transport agent non-derived from coffee” (ISO/FDIS 3509).

Figure 2 Key technological steps to obtain coffee concentrates, instant coffee and RTD coffee beverages.
Packaging and the Shelf Life of Coffee 7

Europe represents the world’s largest instant coffee consumer market (sales market share 37%), followed by China (sales market
share 12%) and the US (sales market share 11%) (www.reuters.com/brandfeatures/venture-capital/article?id¼81988). Instant
coffee is obtained from coffee concentrates by further dehydration to reach a final moisture content below 5%. Spray drying and
freeze drying are the two operations usually applied for this purpose. Spry drying is generally followed by an agglomeration process,
generating larger particles that can better dissolve in the consumer’s cup (Bassoli, 2019). Instant coffee (e.g. powder or granulated) is
sold either alone or in combination with other ingredients to obtain ready-to-prepare beverages, such as Cappuccino.

Quality Loss of Instant Coffee During Storage


Instant coffee is very susceptible to volatile oxidation and flavor release. For this reason, considerations on coffee staling previously
made for whole and ground roasted coffee are also valid for instant coffee. Indeed, the oxygen concentration in the atmosphere in
contact with the product is the determining factor affecting the rate of oxidative reaction during storage. Thus, its concentration should
be reduced as much as possible to increase the product shelf life. Similar considerations hold for light exposure, which is well known to
further promote oxidative reactions. Moreover, being hygroscopic, instant coffee is also susceptible to the action of moisture which, as
previously described, affects volatile liquid partition. An increase in moisture content to 7%–8% is reported to be responsible for
instant coffee “caking”, turning flowing powders or granules into a pastry or solid mass (Clarke, 2001). In the literature it is reported
that instant coffee maintains its original quality for years if the moisture content is kept lower than 4%–5% w/w.
Based on these main alterative events, changes in headspace volatiles determined by instrumental analysis or by sensory analysis
are expected to be optimal indicators to monitor quality depletion of instant coffee during storage. Unfortunately, on this topic
there is very little literature and no specific gas-chromatographic indices are proposed to monitor quality depletion of instant coffee
during storage. On the other hand, physical changes associated with moisture uptake during storage can be followed by direct
measurement of water content or by assessing water activity of the product. At the same time, the physical changes in the particles
(e.g. flowability, stickiness) can also be used as possible indicators of product failure during storage.
Table 4 summarizes the main indices that can be used to monitor instant coffee quality changes during storage.

Packaging of Instant Coffee


Instant coffee has been commercialized for many years and is mainly packaged in glass jars or tinplate cans of various shape. These
materials have high barrier properties against both moisture and oxygen. To assure a complete moisture/oxygen barrier, a screw cap
of metal or plastic is sealed on the rim of the container (Clarke, 2001). Today flexible laminated materials are also employed to
produce multiple or single doses (Alves and Bordin, 1998). In all cases, to assure high product quality during storage, with a final
shelf life of about 18–24 months, the headspace of the container is generally saturated with nitrogen to decrease oxygen below 1%.
Moreover, the possible effect of light on product quality packaged in see-through containers should not be underestimated. This is,
for instance, the case with glass containers, beloved by consumers for the possibility to clearly appreciate product color, but very
dangerous for the product due to the triggering effect of light on oxidative reactions. Table 5 summarized the main packaging mate-
rials used for instant coffee.

Table 4 Possible indices of quality changes during storage instant coffee

Indices Reference

Sensory indicators De Oliveira et al. (2009)


Water activity Anese et al. (2005)
Moisture uptake Alves and Bordin (1998); Alves et al. (2000)
Particle changes Saragoni et al. (2007)

Table 5 Main packaging materials for instant coffee. Barrier properties against oxygen and moisture, potential recyclability and head space
atmosphere are also reported

Package Material Head space Barrier properties Recyclability

Jar Glass Modified atmosphere High Total


Can Tinplate Modified atmosphere Total Total
Aluminum multi layered materialsþ external cardboard Modified atmosphere High None
Bag/single use sachet Flexible laminated aluminum Modified atmosphere High None
8 Packaging and the Shelf Life of Coffee

Coffee Concentrates and Beverages


Coffee concentrates are mainly used as semi-manufactured products to be further processed into instant coffee or coffee beverages
(Fig. 2). It should be noted that coffee concentrates are not only used at industrial facilities but are also packaged and sold as
flavoring ingredient for different products (e.g. ice cream and chocolate derivatives).
In recent years, ready-to-drink (RTD) coffee has been dramatically redefined by the coffee industry. Ready-mixed coffee bever-
ages, coffee jelly beverages, and coffee-milk admixtures are only some examples. Moreover, fortified coffee drinks consisting of
instant coffee, with added proteins, carbohydrates, vitamins or minerals as supplements, have appeared on the market. On the basis
of geography, North America and Europe occupy pioneering and dominant market positions. However, the emerging markets of
Asia-Pacific and South America present a very high potential volume.
The starting material for production of RTD coffee beverages is mainly coffee concentrate with added water, flavorings and stabi-
lizing ingredients. The mixture is then subjected to pasteurization and refrigerated storage or sterilized for ambient storage. In fact,
microbial spoilage could critically affect the safety of these products, being low-acid and with high water activity.
In recent years, alongside traditional RTD beverages obtained through hot extraction, the new method of cold extraction is gain-
ing popularity in the market, especially among younger consumers. Cold brewing is carried out at room temperature (20 to 25  C or
lower) over a longer period than traditional hot brewing methods, with typical steeping times ranging from 8 to 24 hours. Cold
brew coffee can be made by percolation or infusion (Cordoba et al., 2019). Also, in this case, after industrial extraction, the product
can be concentrated by water removal to be converted into a flavoring ingredient or a semi-processed material. The latter might be
further processed and customized by adding other ingredients to obtain cold brew RTD beverages, which need a sanitization phase
before marketing.

Quality Loss of Coffee Concentrates and Beverages During Storage


Microbial growth might play a critical role in pasteurized coffee brews and coffee-based beverages. In these products, the growth of
alterative microorganisms could be responsible for quality depletion during refrigerated storage. When microbial growth is not an
issue, RDT coffee beverages are generally prone to chemical reactions, leading to an increase in perceived sourness. These changes are
accompanied by a pH decrease, corresponding to an increase in titratable acidity. Quality depletion of liquid coffee starts imme-
diately just after brewing. It was suggested that the pH decrease could be a consequence of complex reactions, probably related
to non-enzymatic browning pathways involving carbohydrates and amino acids. Additional mechanisms involving lactone hydro-
lysis could also contribute to a pH decrease (Clarke, 1989a,b).
Beside pH changes, oxidative reactions could also be responsible for quality depletion, especially for long-life products stored at
ambient temperature. In fact, coffee compounds as well as other added ingredients (flavors, dairy derivatives and colorants) could
undergo oxidation during storage.
Typical indicators of quality depletion for this class of product are headspace volatile profile, pH, and sensory attributes.
Consumer acceptability can also be used (Nicoli et al., 1989; Dalla Rosa et al., 1990; Manzocco and Lagazio, 2009).

Packaging of Coffee Concentrates and Beverages


Coffee concentrates are mainly packed in large-size containers for further use in the food industry as ingredients for different coffee
derivatives or other food products (Table 7). Thus, they are mainly packed in bag-in-box plastic containers.
More variability is expected for ready-to-drink coffee beverages. Pop-up aluminum cans are a popular option. Further coffee
drinks are available in plastic cups with different shapes. Some of these can be instantaneously heated or cooled thanks to the pres-
ence of an inside cavity containing endothermic or exothermic salts and water separated by a thin layer. By breaking this layer and
shaking the container, salts and water mix, releasing or adsorbing heat. Some manufactures also offer liquid coffee in plastic bottles
or bag-in-box packages to those consumers who need to purchase relatively large volumes. Tetra Pak cartons are also available.

Shelf Life Assessment of Coffee Products

The progressive deterioration of coffee products quality limits their shelf life. This event is inevitable, being the result of the dynamic
nature of coffee derivatives and, depending on their specific characteristics, is accelerated by inadequate distribution or storage

Table 6 Possible indices of quality changes during storage of coffee concentrates and beverages

Indices Reference

Microbial growth -
pH Manzocco and Nicoli (2007)
Titratable acidity Yamanashi et al. (1992)
Headspace volatiles -
Sensory indicators Manzocco and Lagazio (2009); Perez-Martinez et al. (2008)
Packaging and the Shelf Life of Coffee 9

Table 7 Main packaging materials of coffee concentrates and beverages. Barrier properties against oxygen and moisture
and potential recyclability are also reported

Package Material Barrier properties Recyclability

Bottle Glass High Total


Plastic materials Variable depending on the material Variable depending on the material
Pouches or bag-in-box Plastic material High None
Can Aluminum Total Total

conditions such as high temperature, light or relative humidity. Coffee products not having the expected sensory properties, or
exceeding the expiration date declared on the label, are likely to be rejected by the consumers, becoming waste. The assessment of
the time needed for coffee quality to reach a limit value for consumption is thus essential to guarantee the optimal use of the
product and avoid waste. Food shelf life has been defined as the finite length of time, after production and packaging, during
which the product retains a required level of quality under well-defined storage conditions (Nicoli, 2012). Packaged food,
such as coffee derivatives, not only has a primary shelf life but might also have a secondary shelf life. The latter is defined as
the period of time after package opening during which the coffee product maintains an acceptable level of quality (Nicoli
and Calligaris, 2018).
The implementation of adequate protocols of primary and secondary shelf life assessment is thus crucial to guarantee that coffee
products reach the consumers at a quality level sufficiently high to hinder discarding decisions. The general structure of the shelf life
assessment protocols for coffee products can be derived from basic food shelf life testing with some adaptation, depending on the
nature of the coffee products. In fact, given the wide range of coffee products available on the market, their shelf life testing should
be carefully designed by taking into account the peculiarity of each type of product. Table 8 shows the consequential steps needed to
generate reliable shelf life data by applying real time shelf life testing or accelerated shelf life testing.

Table 8 Shelf life assessment protocol

Coffee products
Coffee concentrates and
Shelf life assessment steps Roasted coffee Instant coffee beverages

1. Define the main critical event Oxidative reactions Oxidative Nonenzymatic browning
Volatile loss reactions Ester hydrolysis
Physical collapse Volatile loss
Oxidative reactions
2. Identify the quality indicator (I) Headspace Headspace pH
volatiles volatiles Titratable acidity
Sensory Moisture uptake Sensory sourness
descriptors Sensory indicators Headspace volatiles
3. Define the shelf life acceptability limit (Ilim) The shelf life acceptability limit is mainly a company choice.
There are no compulsory indications on coffee quality limits.
Regulation limits of contaminant migration from packaging are available.
4. Perform the shelf life tests under actual or temperature accelerated Collection of the values of the critical indicator (I ) for samples stored at:
conditions 4  C (chilled coffee products)
20  C (shelf stable coffee products)
20–50  C (shelf stable coffee products under accelerated conditions, ASLT)
5. Identify the reaction order The critical indicator (I ) mostly changes during storage according to
a straight line (Zero order) or an exponential relation (First order)
6. Perform statistical analysis to calculate the rate of quality depletion (k) The effect of storage time (t) on critical indicator (I ) is generally estimated by
classic kinetic analysis and expressed as reaction rate (k):
Zero order I ¼ kt þ Io
First order lnI ¼ kt þ lnIo
The effect of temperature on reaction rate in ASLT is estimated by Arrhenius
equation, and expressed as Activation Energy (Ea):
lnk ¼  ERa T1 þ lnk0

7. Calculate shelf life (SL) Shelf life is computed substituting the acceptability limit in the shelf life
equation:
Zero order SL ¼ IlimkIo
First order SL ¼ lnIlimklnIo
8. Validate shelf life estimate by product monitoring in the food chain Comparison of values of quality indicators in food during storage on the
market with those estimated in the lab
10 Packaging and the Shelf Life of Coffee

Step 1. Define the main critical event


The first step of the shelf life assessment protocol is aimed at identifying the most critical event leading to coffee product quality
decay. As previously discussed, most coffee products are shelf-stable foods with a medium to long shelf life, prone to the develop-
ment of chemical reactions such as oxidation, volatile loss and ester hydrolysis.
Step 2. Identify the critical indicator (I)
The evolution of alterative phenomena is generally monitored by following the changes in the most important chemical and
sensory indicators. A detailed description of possible indices to be followed for shelf life assessment is reported in
Tables (Tables 1, 4 and 6).
Step 3. Define the shelf life acceptability limit (Ilim)
Once the proper indicator of the quality depletion of coffee products has been selected, the third step of the shelf life assess-
ment protocol requires the definition of the acceptability limit. The latter is the value of the critical indicator distinguishing prod-
ucts which are still acceptable for consumption from those that are no longer acceptable (Manzocco, 2016). Despite its
apparently intuitive nature, the acceptability limit is often a vague boundary: it should be selected in correspondence to the
quality level that does not fulfil the consumption standards. In the case of coffee products, consumption standards are not re-
ported in the regulations but are consumer driven. The acceptability limit is often inevitably chosen by the company based
on discretional considerations, taking into account the risk of sensory default but also aspects relevant to delivery system and
business, such as the risk for product recalls or inadequate turnover of the product on the retail shelves. The evaluation of coffee
acceptance limits is increasingly based on sensory studies involving consumers (Hough et al., 2003, 2004; Ramirez et al., 2001;
Cardelli and Labuza, 2001). In this regard, the methodology providing comprehensive information to determine acceptability
limit and shelf life using consumer data is based on survival analysis of product acceptability (Gacula and Kubala, 1975; Gacula
and Singh, 1984; Hough et al., 2004). According to the industrial policy, the food company can choose more or less risk by select-
ing as the acceptance limit, the percentage of consumers who reject the product. Conventionally 25%–50% consumer rejection is
generally adopted as an acceptability limit. However, it should be noted that the evaluation of consumer acceptability is a time-
consuming and expensive process, requiring large sample sizes and large consumer numbers to run the experiments. As a conse-
quence, acceptability studies are hard to apply to routinely assess shelf life. To meet industrial needs, consumer acceptability
limits can be correlated to instrumental and sensory attributes, which are easily measured during product storage. For instance,
it has been demonstrated that a 50% consumer rejection of a coffee brew was reached when its pH decreased to 5.14 (Manzocco
and Lagazio, 2009). Similarly, a 50% consumer rejection of roasted ground coffee was observed to correspond to a 60% reduc-
tion of the initial headspace volatile area (Anese et al., 2006).
Although in most cases, unacceptability of coffee products is the result of the intrinsic instability of coffee products, in some
cases, it might also derive from the interaction between product and package. For instance, the migration of plastic constituents
from packaging materials into the product during storage could reach values exceeding those reported in the regulations. In this
case, the acceptability limit is no longer a company choice but is selected in strict adherence to legal requirements for food consump-
tion. In other words, a value of contaminant migration much lower than that indicated by the regulation is generally selected as an
acceptability limit. In this way, the risk that products with excessive contamination levels might be present in the market is signif-
icantly reduced.
Step 4. Perform the shelf life test under actual or temperature-accelerated conditions
In this phase of the shelf life assessment protocol, the changes of the selected quality indicators (I) are evaluated as a function of
time (t) in order to determine the reaction order (Step 5) and the reaction rate (Step 6) by the application of the classic kinetic
approach. Collection of experimental data during product storage can be performed under actual (real time) or accelerated
(ASLT) conditions.
Real Time Shelf Life Tests
In these tests the product is stored under reasonably foreseeable storage conditions. The basic requirement is that the environ-
mental conditions during sample storage (e.g. temperature, moisture, oxygen concentration, light) are kept constant and as close as
possible to those actually experienced by the product on the market shelves. For instance, shelf stable coffee products are stored at
20–25  C and chilled beverages at 4–6  C. In all cases, if the product is packaged in a see-through material, the role of light exposure
should not be neglected, and samples should be stored under the typical light intensity of the market shelves (800 lux).
Storage under actual conditions is potentially applicable to any coffee product but is more profitable in the case of products
for which quality decay occurs in a relatively short time (<3–4 months). This often occurs for secondary shelf life of coffee
products.
Accelerated Storage Shelf Life Tests (ASLT)
If quality depletion occurs over a long time, speeding up the shelf life assessment process is often requested to reduce the time
needed for the tests and to fit industrial needs. In this case, samples are stored under environmental conditions that speed up quality
deterioration, and reaction kinetics are used to extrapolate reaction rates at actual storage conditions (Labuza and Schmidl, 1985;
Labuza and Riboh, 1982; Calligaris et al., 2019). Such tests are known as accelerated shelf life tests (ASLT) and are particularly useful
to study the primary shelf life of coffee products, which is typically long. Although a number of different environmental factors
accelerating food quality depletion are known, temperature is the only one to be extensively used in shelf life tests of coffee
products.
Packaging and the Shelf Life of Coffee 11

Step 5. Identify the reaction order


Data collected, either under actual or accelerated conditions, are initially plotted as a function of storage time to establish the
reaction order. A seemingly linear pattern of points is generally observed for indices describing chemical or sensory oxidation of
coffee products. This linear patter indicates that the zero order kinetics is adequate. If the pattern exhibits a curvature, as often
observed for coffee products prone to pH lowering, kinetic functions of higher order should be considered. In these cases, the
plot on a logarithmic scale generally applies, and a first order kinetic function can be used.
Step 6. Perform statistical analysis to calculate the rate of quality depletion (k)
When the reaction order has been identified, linear regression analysis is carried out to obtain the values of the reaction rate (k) of
quality depletion. For instance, Fig. 3 shows the values of total volatile compounds in the headspace of roasted coffee at increasing
storage time during simulation of domestic usage at 25  C and 36 ERH% (data from Anese at al., 2006). Data of the original gas
chromatographic signal were expressed as a percentage and plotted as a function of storage time.
Since the plot clearly shows that the pattern is linear and that data can be elaborated according to zero-order kinetics (Step 5),
linear regression was carried out and provided the coefficient parameter showed in Fig. 3. The percentage of total head space vola-
tiles (Vt) during time (t) of coffee domestic storage after package opening can be thus described by the following equation:
Vt ¼  2:13t þ 89:73
where 2.13 is the value of the apparent reaction rate (k) and 89.73 is the estimated value of the intercept (Vo).
If the test has been carried out under temperature accelerated conditions (20–50  C), rate constants for each storage temperature
are plotted to describe the relationship between rate constant and temperature. In particular, logarithmic values of reaction rates are
plotted versus 1/temperature (measured in K) to estimate the parameters of the Arrhenius equation. The pattern is generally linear
and values of frequency factor (ko) and activation energy (Ea) are estimated by linear regression. In this regard, accelerated shelf life
tests of roasted coffee stored under air showed that the temperature dependence of headspace volatile loss rate was well described by
the Arrhenius model (Nicoli et al., 1993) with apparent activation energy allowing consistent speeding up of the alterative event. An
example of the application of this methodology is shown in Fig. 4, with reference to hexanal formation in ground roasted coffee
stored in air.
Hexanal formation quickly proceeded at storage temperatures between 30 and 50  C (Fig. 4A). By contrast, the oxidation rate
at 20  C was definitely slow, requiring a much longer testing time for accurate assessment. Reaction rates in the accelerated
temperature range (30–50  C) were calculated according to zero-order kinetics and expressed as logarithmic values in an Arrhe-
nius plot (Fig. 4B). The parameters of the Arrhenius equation, obtained by regression analysis, can be used to predict the reaction
rate at any temperature in the experimental range tested and even at its boundary. In particular, the value of the reaction rate at
20  C, which is the actual storage temperature of the product, was estimated to be about 1100 A.U./day. Although this procedure
allows the shelf life testing time to be significantly reduced, it is recommended to confirm predicted reaction rates at actual
storage conditions by comparison with experimental ones since deviations from the linear behavior of the Arrhenius plot could
be present.
The Arrhenius equation has been demonstrated to hold also for hydrogen ion formation in coffee brews and concentrates
(Manzocco and Nicoli, 2007). By contrast, when roasted coffee was packed in modified atmospheres, the magnitude of the activa-
tion energy was quite low, emphasizing the limited temperature sensitivity of the product and thus the need to speed up alterative
events using accelerating factors other than temperature, such as oxygen concentration.
Step 7. Calculate shelf life
Once the shelf life limit (Ilim) and the reaction rate (k) are available, such data can be used to compute the shelf life value by
integrating them into the relevant kinetic models (Step 7).

Time Total volatile


(days) area 120 Experimental
Estimated
Total headspace volatiles

100
(%) 80
60
0 100
(%)

40
2 79 20
5 68 0
0 10 20 30
7 79 Time (days)
12 63
16 58 Coefficients SE Stat t p-Value
20 53 Intercept (%) 89.73 3.88 23.11 7,2·10-8
Rate constant (%/day) -2.13 0.26 -8.24 7,54·10-5
22 42
26 32
Figure 3 Percentage of total volatiles in the headspace of roasted coffee during simulation of a domestic usage at 25  C and 36% ERH%, and
results of regression analysis.
12 Packaging and the Shelf Life of Coffee

A 1600000 B 10
50 °C k= 14340 A.U./day
1400000 9.5

Head space hexanal (A.U.)


1200000 9

Lnk(A.U./days)
1000000 8.5

800000 8
40 °C k= 5390 A.U./day
600000 7.5
400000 30 °C k= 2641 A.U./day
7 k predicted at 20 °C
200000 20 °C based on Arrhenius equa on:
6.5 Lnk= -8262,6·(1/T) + 35,097
0
6
0 20 40 60 80 100
0.003 0.0031 0.0032 0.0033 0.0034 0.0035
Time (days) 1/T (K)
Figure 4 Calculation of rate constants and Arrhenius plot of hexanal formation in ground roasted coffee packaged in air (Melchior, 2019
unpublished data).

For instance, in the case of secondary shelf life of roasted ground coffee (Fig. 3), shelf life (SL) can be calculated according to the
following expression (zero-order equation):
Vlim  Vo
SL ¼
k
where Vlim corresponds to the acceptability limit of total headspace volatiles. By selecting a 60% decrease of total volatile decrease as
the acceptability limit, the shelf life data can be estimated as equal to 14 days (Cardelli and Labuza, 2001; Anese et al., 2006). It is
noteworthy that this shelf life data is only relevant to the roasted coffee stored under the environmental conditions applied during
the shelf life test (25  C and 36 ERH%). If the product is expected to be stored under environmental conditions other than those
considered during the test, the SL estimate would not be as accurate. This means that the acceptability limit of a 60% reduction of
total volatiles might be reached in shorter or longer times than estimated. Proper validation of parameters estimated by monitoring
both environmental conditions and volatile changes under real conditions is thus needed.
Step 8. Validate shelf life estimate by product monitoring in the food chain
The shelf life estimates deriving from laboratory tests are generally validated by comparison of the expected evolution of the
quality indicators with those actually measured in the coffee product collected from the food chain. Further information is derived
from recalls and complaint data and allows development of a historical experience of the producer about the product shelf life.
These data can be used to adapt shelf life tests to better mimic the conditions experienced by the product in the market, and to
confirm or correct the expiration date communicated on the label. The greater the historical experience of the producer, the
more effective will be the integration of the shelf life assessment protocols into the quality management system of the company,
guaranteeing both the reputation of the company brand in the market and the optimal use of the product by consumers.

Consideration on the Secondary Shelf Life of Coffee Products


The secondary shelf life of food is an underestimated topic. As previously defined, it is the period after pack opening during which
the product maintains an acceptable quality level. Dried coffee products are an exemplary case on this topic, because their use after
pack opening is spread over a significant length of time at domestic or catering level. Quality issues emerging after pack opening are
mainly related to the changes of the pack atmosphere composition, due to the entrance of oxygen and/or moisture into the pack,
and concomitant escape of volatile compounds. These events could rapidly lead to product quality depletion. The dramatic effect of
pack opening can be well understood considering the difference between primary and secondary shelf life of ground roasted coffee.
Based on data reported by Anese et al. (2006), the estimated secondary shelf life is about 15 days while primary shelf life, as reported
by producers, is 18–24 months.
The case of RTD coffee beverages is different in that microbial growth could become the most important issue when the product
package is opened and its consumption is incomplete. In fact, when the package of a pasteurized/sterilized coffee beverage is
opened, microbial contamination is likely to occur and quality depletion might proceed according to mechanisms other than those
expected in the closed package. In this case, the secondary shelf life is generally around 2–3 days.
Considering the consumer handling of coffee products after opening, the experience of a bad coffee cup could lead on one side to
product wasting and on the other to loss of trust in the brand. Notwithstanding the issues associated with pack opening, no infor-
mation of product storage life after pack opening is generally provided on the label. In this regard, the provision of label informa-
tion would guide the chain operators to optimize stock rotation and the consumer to better manage the household storage of
products, reducing overall waste.
Packaging and the Shelf Life of Coffee 13

Conclusions

Coffee comprises a number of different products ranging from whole and ground roasted coffee to a wide variety of convenience
and semi-manufactured products such as instant coffee, coffee concentrates and ready-to-drink coffee beverages. Each of these prod-
ucts has specific characteristics and thus different requirements for packaging solutions. The choice of packaging and relevant pack-
aging techniques should result from matching their properties with the protection requirements of the coffee product during both
primary and secondary shelf life. The knowledge of typical material parameters, such as permeability to moisture or gases, is not
enough. Interactions between packaging and coffee products under defined conditions of environment and consumer use are often
very complex. For this reason, the selection of the optimal packaging requires the ability to estimate coffee product shelf life in the
different materials. In the light of the strong driving force of packaging sustainability, novel materials are expected to appear on the
market. A great deal of work and long times will be needed to assess their suitability for coffee products, with high risks of nonop-
timal packaging solutions or overpacking. The ability to make quick predictions by accelerated shelf life models will be crucial to
provide environmental benefits with no detriment to product quality.

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