OOD Ntegrity Andbook: Guide To Food Authenticity Issues and Analytical Solutions
OOD Ntegrity Andbook: Guide To Food Authenticity Issues and Analytical Solutions
OOD Ntegrity Andbook: Guide To Food Authenticity Issues and Analytical Solutions
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Coffee
Jean-François Morin*, Eric Jamin, Sophie Guyader, Freddy Thomas
Eurofins Analytics France, Nantes, France
*E-mail corresponding author: JeanFrancoisMorin@eurofins.com
https://doi.org/10.32741/fihb.16.coffee
Coffee
A great variety of coffee products can now be purchased. International coffee trade is conducted
almost exclusively in green coffee. However, consumers are nowadays offered roasted coffee
beans, roasted and ground coffee, as well as liquid and dried coffee extracts (soluble coffee).
Furthermore, coffee can be mixed with coffee substitutes, and also sold as roasted and ground
blends or as dried extracts. Whole-bean roasted coffee may also be soaked with liquid flavouring
agents to produce flavoured coffees. Finally, dried coffee extracts already containing milk solids
(café au lait, cappuccino) exist on the market. Decaffeinated forms of each of these coffee
products are also available.
The different varieties of coffee bean and the region where the coffee is grown may give rise to
products of different qualities that are more or less popular with the consumer. This in turns leads
to price differences on the market and the potential for adulteration or misrepresentation by a
dishonest trader. A popular component of the Western diet, coffee is also an important
commodity in international trade upon which the economies of a number of countries are
particularly dependent. In 2010 the International Coffee Organization (ICO) estimated total coffee
sector employment at about 26 million persons in 52 producing countries[4]. Thus, the coffee
industry itself has devoted considerable time and effort to ensuring both the quality and
authenticity of its product, and to developing suitable analytical techniques for this purpose.
In the last 30 years, the coffee market has seen the emergence of an increasing number of
initiatives related to fair-trade and sustainability. Often marked with a label on the coffee
packaging, these labels certify the sustainability of coffee production and the respect of
smallholder producers by improving their conditions of trade (e.g. more equitable and more stable
prices). In the coffee market, most extended programmes are UTZ Certified and the Rainforest
Alliance, which merged early 2018, and the Max Haavelar Foundation. According to Fairtrade
International, fair-trade coffee farmers produced an estimated 560 900 tonnes of coffee in 2015
(approximately 6 % of the worldwide production).
1. Product Identity
1.1. Definition of the product and manufacturing process
Green coffee may be produced by either a wet or dry process. The wet process involves washing
the coffee cherries and transferring them to depulping machines which remove the outer skin and
most of the pulp. This process leaves some of the pulp mucilage on the parchment shells which
encase the coffee bean and this remaining mucilage is fermented and washed away with clean
water. The beans are then dried and the inner husk known as 'parchment' is broken by rollers and
removed. Further rubbing removes the film or 'silverskin' which closely adheres to the coffee bean.
The dry process involves drying the fresh ripe cherries in the sun for up to three weeks. The dried
coffee cherries are dehulled mechanically to remove the outer skin, pulp, 'parchment' and the
'silverskin' to leave the clean, naked, green coffee beans.
Coffee is usually traded as green coffee beans, a state in which they can be kept without loss of
quality or taste. It is roasted and further processed in the purchasing country. Roasting brings out
the aroma and flavour that is locked inside the green coffee beans. The roasting process involves
the heating of the green beans at about 200 °C, followed by fast cooling to stop the process. Once
roasted, coffee should be used as quickly as possible before the fresh roast flavour begins to
diminish.
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Coffee
Instant coffee (soluble coffee) is also produced in the coffee growing countries and may be traded
packed ready for retail sale or in bulk for re-packaging in the country of receipt for national
consumption or for further export. Instant coffee is the dried water-extract of roasted, ground
coffee. Roasted, ground coffee is placed into columns known as percolators through which hot
water is fed in a counter-current process. The extract is further concentrated and may be traded in
bulk as such or dried to produce soluble coffee solids. Instant coffee is sold in three forms, which
relate to the drying process of the soluble coffee extract. Instant coffee powder is formed by spray
drying the extract; coffee granules are formed by agglomerating this powder with steam; and
freeze-dried coffee is formed by removing moisture from the extract under vacuum (sublimation)
at much lower temperatures than spray drying. Freeze-drying is more energy expensive but is
gentler on the product as less heat is applied to evaporate the water content. Consequently,
freeze-drying is used for the finer and more expensive blends of instant coffee.
Decaffeinated coffee is produced from green beans. Three different extraction processes slightly
differing from each other are in use in the industry. Basically a solvent is circulated around the
water soaked beans and this causes the caffeine to be released. The most widely used and less
costly is extraction with an organic solvent such as methylene chloride (also known as
dichloromethane) or ethyl acetate, an ester that is found naturally in fruits and vegetables. The
second method is water processing: water is used as a solvent to extract the caffeine. In the third
approach, carbon dioxide in supercritical state under a pressure of 250 to 300 bar circulates
through a bed of green beans. At the end of the process, caffeine content is usually reduced from
1–2 g% to 0.02–0.3 g% [5].
The ICO was formed in 1962 under the auspices of the United Nations. It is a inter-government
body comprising 51 coffee importing and exporting countries which aims through international co-
operation on trade in coffee to achieve economic diversification and development of coffee-
producing countries, increased coffee consumption, price stabilisation and improved economic
relations between coffee exporting and importing countries. The ICO is well regarded for its
statistical services and its role as the international forum for discussing all issues affecting the
world coffee market. It also co-ordinates a number of projects (most of which deal with marketing,
pest/disease/quality problems or sustainability) and holds seminars on issues such as the
environmental aspects of coffee production and the use of the futures market.
The International Coffee Agreement 2007 is the legal agreement which sets out how these
objectives will be met [6]. In this document, the different coffee products are defined for
harmonising data collection, statistics and trade among producing and importing countries. On the
other side, the International Standard Organisation has issued a standard “Coffee and coffee
products – Vocabulary” (ISO 3509:2005) [7] also for setting the definitions of coffee products. The
same terms, such as “Roasted coffee” or “Decaffeinated coffee” can be found in both documents,
but definitions are largely consistent. Roughly ICO definitions are more statistically oriented
whereas ISO focuses more on quality and process.
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Coffee
Table 1: Comparison of the definition of coffee and coffee products between ICO and ISO
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Among these standards, two of them have a special application to instant coffee authenticity. The
standard “Instant coffee - Criteria for authenticity” (ISO 24114:2011) [8] specifies criteria for
authenticity of soluble (instant) coffee. Its purpose is to identify adulterated soluble coffee,
defined as a “product prepared by the co‐extraction or the separate extraction of roasted coffee
beans and of raw or roasted materials other than coffee beans, where the product is sold as pure
soluble coffee and the addition of the non‐coffee bean material is not declared on the label”. The
aim is to avoid incorrect declarations that adulterated products with cheaper coffee substitutes
are 100 % pure soluble coffee. The standard focuses on two different parameters: total glucose
and total xylose, the values of which must not exceed certain limits (respectively 2.46 % and
0.45 %) for the instant coffee sample to be declared authentic.
The standard is based on a standardised method looking at the carbohydrate content of the
instant coffee, under the reference “Instant coffee - Determination of free and total carbohydrate
contents - Method using high-performance anion-exchange chromatography” (ISO 11292:1995)
[9]. The free and total carbohydrate profiles in soluble coffee are determined by anion exchange
chromatography with pulsed amperometric detection (AE-PAD).
For roasted coffee, the German standard method “Analysis of coffee and coffee products -
Determination of 16-O-methyl cafestol content of roasted coffee - HPLC-method” (DIN
10779:2011) [10] can also be used for authentication purposes. It is used to quantify the amount
of 16-O-methylcafestol (16-OMC) in roasted beans originally, even if applications to green coffee
beans and coffee brews have also been described in the literature [11]. It is based on the
observation that 16-OMC is present exclusively in Robusta.
1.2.2. EU legislation
Beyond general regulations on food products, such as the General Food Law (Regulation EC
178/2002), the European Union has set up several regulations dealing with coffee products.
The general EU Regulation 1169/2011 [12] on the provision of food information to consumers,
combines two Directives into one legislation: 2000/13/EC - Labelling, presentation and advertising
of foodstuffs, and 90/496/EEC - Nutrition labelling for foodstuffs. Among other themes, it deals
with the labelling of origin. No specific rules have been set up for coffee, the general principle that
“information shall not be misleading” applies. Voluntary provenance labels (i.e. indication where
the green coffee was grown) can be made in relation to product claims such as ‘100 % Brazilian
coffee’.
This regulation also stipulates a list of foods, including the following coffee products, which are
exempted from the requirement of the mandatory nutrition declaration:
● Products covered by Directive 1999/4/EC of the European Parliament and of the Council
of 22 February 1999 relating to coffee extracts and chicory extracts,
● Whole or milled coffee beans and whole or milled decaffeinated coffee beans.
Directive 1999/4/EC [13] relating to coffee extracts and chicory extracts determines which
substances may be added during manufacturing of these products, lays down common rules
concerning the packaging and labelling of such extracts and specifies the conditions under which
particular designations may be used for some of these products. It simplifies the legislation
previously regulated by Directive 77/436/EEC.
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Coffee
It defines coffee extracts as “the concentrated products obtained by extraction from roasted
coffee beans using only water as the medium of extraction and excluding any process of hydrolysis
involving the addition of an acid or a base”.
In particular it stipulates that “coffee extract must contain only the soluble and aromatic
constituents of coffee”, apart from those insoluble substances which it is technically impossible to
remove, and insoluble oils derived from coffee.
It controls the composition of three types of coffee extracts which differ in terms of their coffee-
based dry matter content:
● Dried coffee extract: not less than 95 % by weight,
● Coffee extract paste: from 70 % to 85 % by weight,
● Liquid coffee extract: from 15 % to 55 % by weight.
Liquid coffee extract is specifically allowed to contain edible sugar provided the sugar content in
the final product does not exceed 12 % by weight. The Directive does not permit coffee extract in
solid or paste to contain any substance other than those derived from its extraction.
This Directive also states that the term 'decaffeinated' can only be applied to coffee extracts which
have an anhydrous caffeine content of not more than 0.3 % by weight of its coffee-based dry
matter content.
The Directive does not cover roast and ground coffee.
According to Directive 2009/32/EC [14], solvents can be used for decaffeination of coffee in the
European Union. There are maximum residue limits restrictions for the extraction solvents such as
methyl acetate (20 mg/kg in the coffee), dichloromethane (2 mg/kg in the roasted coffee) and
ethylmethylketone (20 mg/kg in the coffee). In the United States, according to the FDA, methylene
chloride may be present in coffee as a residue from its use as a solvent at a level not to exceed 10
parts per million in decaffeinated roasted coffee and in decaffeinated soluble coffee extract
(instant coffee) [15].
Directive 2002/67/EC [16] on the labelling of foodstuffs containing quinine,and caffeine sets up
specific rules for protecting consumers and providing them with clear information on the presence
of these compounds.
Where a beverage which is intended for consumption without modification, or after reconstitution
of the concentrated or dried product, contains caffeine, from whatever source, in a proportion in
excess of 150 mg/l, the following message must appear on the label in the same field of vision as
the name under which the product is sold: "High caffeine content". This message shall be followed
by the caffeine content expressed in mg/100 ml.
However, this obligation does not apply to beverages based on coffee, tea or coffee or tea extract
where the name under which the product is sold includes the term "coffee" or "tea".
One Protected designation of origin (PDO) and one protected geographical indication (PGI) have
been granted by the European Union:
● Café de Colombia (PGI) in Regulation (EC) 1050/2007 of 12 September 2007 [17];
● Café de Valdesia (PDO) in Regulation (EU) 2016/1043 of 15 June 2016 [18].
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Coffee
2. Authenticity issues
2.1. Identification of current authenticity issues
As mentioned previously the two coffee species of commercial importance are Arabica and
Robusta. Producer countries and coffee traders are mainly interested in being able to recognise
the country of origin of coffees, whereas food processors and regulatory authorities are interested
in checking on compliance of the declared composition in commercial blends and in the detection
of adulteration by addition of substitutes or other ingredients
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Coffee
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Coffee
Coffee buyers or roasters are paying more and more attention to the cultivar of the products they
buy. If some introgressed cultivars are preferred because of specific properties, coffee buyers want
to check if purchased coffee batches actually originate from the expected species. Secondly it has
been shown that introgression can have a negative impact on the cup quality of cultivars derived
from the Timor Hybrid. Consequently, coffee buyers or roasters may wish to assess whether the
coffee they are purchasing comes from introgressed varieties [25]. Finally it has been
demonstrated that the variety characteristics are not stable from one harvest to the next making it
necessary to use at least two harvest dates for each variety [26]. Therefore there might be a
concern about procurement quality and stability in time.
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Coffee
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Coffee
coffee. It is based on the observation that 16-OMC is present exclusively in Robusta, whereas
other, more abundant diterpenes, such as cafestol and kahweol, cannot be used for this
discrimination.
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Coffee
models correctly identified all authentic Robusta green coffee beans from Cameroon and Vietnam
and 94 % of those from Indonesia. Moreover, PLS-DA afforded independent models for Robusta
samples from these three countries with sensitivities and specificities of classifications close to
100 % and for Arabica samples from America and Africa with sensitivities of 86 and 70 % and
specificities to the other class of 90 and 97 %, respectively [38].
1 13
Using both H-NMR and C-NMR spectroscopy, it has been shown that metabolite levels in coffee
were significantly different between the Arabica and Robusta species, and secondarily influenced
1
by geographical origins [39]. OPLS-DA models performed on H-NMR data led to a clear separation
of samples according to their origin: fatty acids, chlorogenic acids and lactate and finally acetate
and trigonelline were shown to be the main compounds characterising the American, African and
Asian samples respectively. The analytical approach presented here confirmed the potential of
joint NMR analysis and statistical treatment in coffee authentication [40]. Classification models
were built on aqueous NMR profiles allowing the distinction of 192 coffees on countries or
continents of origin [41]. More precisely, 50 samples of Colombian have been differentiated from
22 Asian, 12 African and 108 other American origins. Although the discrimination was based on the
global fingerprint, fatty acids, acetate and caffeine were identified to having a particular part in the
differentiation. However, some impacts of roasting processes were observed on spectral profile as
well as the post-harvest processes, the ripening periods and the year of harvest.
NIR spectroscopy has also demonstrated its potential in geographical origin authentication. Fourier
transform infrared spectroscopy (FTIR) following solvent extraction permits examination of
molecular variation to distinguish degrees of roast and country of origin, as between Columbia,
Costa Rica, Ethiopia and Kenya [42]. Near-infrared spectroscopy (NIR) has been used to distinguish
geographic origin and genotype of samples grown in Brazil [43].
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Coffee
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Coffee
differentiation of Arabica and Robusta coffees. Indeed, the reference method DIN 10779:2011 [10]
has proven the existing correlation between the 16-OMC concentration and the Robusta rate in
Arabica roasted coffee. In parallel, kahweol was shown to be a key compound in species
differentiation and was considered as a marker of Arabica species, although this compound is
structurally very close to cafestol, compound present in both species.
1
Blend compositions were determined by H-NMR spectral fingerprints with a high accuracy for 56
mixtures in aqueous solution using Orthogonal - Partial Least Square (OPLS) regression models
[53]. This NMR method was proven to be a substitute for the official method because it requires
only limited preparation, thus avoiding the loss of analytes. It was also shown that this technique
could reach low limits of detection and quantification (5 and 20 mg/kg, respectively). This
performance is adequate to detect the presence of Robusta at percentages lower than 0.9 % and
down to 0.2 %, thus lower than the official method by HPLC (about 2 %) [11]. Furthermore, a
recent paper has proven the presence of 16-OMC, a marker of Robusta, in ground roasted Arabica
coffee in the order of 1-2 % [54]. Consequently the limit of quantification for Robusta content
must be defined at 5 % and 10 % respectively in roasted and green Arabica coffee, in order to
avoid false negative results. Moreover, this recent paper detected 2 doubtful market samples of
Arabica coffee with adulterations at levels up to 30 % (w/w) in a panel of 60 retail purchased
coffees using a limit of detection at 1 % and of quantification at 4 % [54].
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Coffee
aroma compounds which are formed during roasting. Arabicas contain (due to their high sucrose
content) considerably higher amounts of steam-volatile furans, hydroxymethylfurfural and some
aliphatic sugar degradation products than Robustas [58]. In a recent paper, a comparison between
1
GC-C-IRMS, GC-MS, and H-NMR was carried out to discriminate coffees from Colombia versus
nearby countries (Brazil and Peru). According to the authors, results show that the quality of the
classifiers depends mainly on the number of variables included in the analysis, which does not
favour GC approaches [59].
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Coffee
racemosa) and one Racemosa (C. racemosa) accession. Six leaf rust resistant Arabica were also
included. Authors concluded that that it is possible to use these SSRs for coffee variety
identification. Single Nucleotide Polymorphism (SNP) has also been studied for identification of
coffee germplasm with good results. A panel of 180 SNPs has been validated on 25 C. arabica and
C. canephora accessions from Puerto Rico [65]. All the Robusta accessions were differentiated, as
well as 10 out the 12 Arabica accessions (the 2 remaining ones were considered as synonymous).
All these tools are available for coffee players to assist in coffee germplasm management, quality
control of planting material propagation, coffee cultivar authentication and protection of varietal
rights in the international coffee community.
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Coffee
5. Conclusion
Coffee authentication is a major concern for the coffee sector. The product itself, once roasted,
ground or processed as instant coffee, can be easily adulterated. Furthermore coffee is one of the
most appreciated and valued food commodities. Extensive research has been carried out on coffee
authentication over the last few decades with the results that robust authentications methods are
now available for the industry throughout the supply chain in order to ensure that genuine
products are delivered to consumers.
The problem of determining the proportion in blends or the adulteration of Arabica with Robusta
has been addressed and there are techniques that provide a good estimation of mixtures.
However, under pressure of changing climate conditions, new varieties are being created by
breeding Arabica and Robusta cultivars, for instance. Current differentiation between these two
species is becoming more and more complex. New knowledge is needed in the future to ensure
accurate results and to avoid false positives.
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