Sensors 2010, 10, 3882-3910; doi:10.

3390/s100403882
OPEN ACCESS

sensors
ISSN 1424-8220
www.mdpi.com/journal/sensors

Review

Metal Oxide Sensors for Electronic Noses and Their Application

to Food Analysis
Amalia Berna

CSIRO Entomology and CSIRO Food Futures Flagship, GPO Box 1700, Canberra ACT 2601,
Australia; E-Mail: [email protected]; Tel.: +61-2-6246-4258; Fax: +61-2-6246-4000

Received: 11 March 2010; in revised form: 12 April 2010 / Accepted: 13 April 2010 /
Published: 15 April 2010

Abstract: Electronic noses (E-noses) use various types of electronic gas sensors that have
partial specificity. This review focuses on commercial and experimental E-noses that use
metal oxide semi-conductors. The review covers quality control applications to food and
beverages, including determination of freshness and identification of contaminants or
adulteration. Applications of E-noses to a wide range of foods and beverages are considered,
including: meat, fish, grains, alcoholic drinks, non-alcoholic drinks, fruits, milk and dairy
products, olive oils, nuts, fresh vegetables and eggs.

Keywords: food; metal oxide semi-conductor sensor; electronic nose; E-nose

1. Electronic Nose and Metal Oxide Semi-Conductor Sensors

The two main components of an electronic nose (E-nose) are the sensing system and the automated
pattern recognition system. The sensing system can be an array of several different sensing elements or
a single device or a combination of both. Volatile organic compounds (VOCs) presented to the sensor
array produces a signature or pattern which is characteristic of the vapor. By presenting many different
chemicals to the sensor array, a database of signatures can be build up. Data analysis and pattern
recognition (PARC) in particular, are also fundamental parts of any sensor array system. There are a
variety of PARC methods available which can be categorized in three classes. The choice of the
method depends on available data and the type of result that is required. Graphical analysis with bar
charts, profiles polar and offset polar plots are simple forms of data treatment that may be used with an
electronic nose. A second way of analysing E-nose signals is by means of multivariate analysis.
Sensors 2010, 10 3883

Multivariate analysis generally involves data reduction. It reduces high dimensionality in a

multivariate problem where variables are partly correlated, allowing the information to be displayed in
a smaller dimension. There are many multivariate techniques to choose from: principal component
analysis (PCA), cluster analysis (CLA), linear discriminant analysis (LDA), partial least squares
(PLS), etc. A third category is based on artificial neural networks (ANN). A neural network consists of
a set of interconnected processing algorithms functioning in parallel. On a very simplified and abstract
level, ANN is based on the cognitive process of the human brain [1,2].
Gas sensors, based on the chemical sensitivity of metal oxide semi-conductors (MOS), are readily
available commercially. They have been more widely used to make arrays for odor measurement than
any other class of gas sensors [1]. Although the oxides of many metals show gas sensitivity under
suitable conditions, the most widely used material is tin dioxide (SnO2) doped with a small amount of
a catalytic metal such as palladium or platinum. By changing the choice of catalyst and operating
conditions, tin dioxide resistive sensors have been developed for a range of applications. Materials
with improved performance with respect to relative humidity variations have been found by empirical
experimentation [3]. Titanium-substituted chromium oxide (CTO) is an example of such a material.
Other available oxide-based gas sensors include zinc oxide (ZnO), titanium dioxide (TiO2) and
tungsten oxide (WO3).
In addition to variations in the composition of MOS sensor materials, the metal oxide film
deposition is an important variable governing sensor performance design [4]. Deposition techniques
include physical or chemical vapour deposition, evaporation and spraying for thin films (6–1,000 nm),
a screen printing and painting for thick films (10–300 µm). While thin film devices offer a faster
response and significantly higher sensitivities, these are much more difficult to reproducibly
manufacture which means that commercially available MOS sensors are often based on thick film
technologies [2].
The sensor usually comprises a ceramic support tube containing a platinum heater coil onto which
sintered SnO2 is coated onto the outside of the tube with any catalytic additives. Gas samples are
sensed by the change in the electrical resistance of the metal oxide semi-conductor. Resistance changes
due to combustion reactions occurring within the lattice oxygen species on the surface of metal oxide
particles [1]. The sign of response (either an increase or decrease in resistance) leads to a simple
classification: gas can be classified as either oxidizing or reducing which means that the oxide can be
classified as p or n type. The n and p type designations indicate which charge carrier acts as the
material's majority carrier. N types are semi-conducting materials, which are doped with atoms capable
of providing extra conduction electrons to the host material. This creates an excess of negative (n-type)
electron charge carriers. P type semi-conductor (p for positive) is obtained by carrying out a process of
doping, that is adding a certain type of atoms to the semi-conductor in order to increase the number of
free charge carriers (in this case positive). For p type oxides, an increase in the resistance is found in
the presence of reducing gases, while the resistance decreases in response to oxidizing gases; n-type
oxides show opposite behavior [3]. Examples of n type oxides are SnO2 and WO3; and a p-type oxide
is CTO.
An electronic nose can detect and estimate odors quickly though it has little or no resemblance to
animal noses. Sensors used in E-noses are less independent and are more narrowly tuned to certain
VOCs, compared with olfactory receptors from invertebrate animals like fruit flies [5]. Although MOS
Sensors 2010, 10 3884

sensors respond to a broad range of volatiles, they have higher affinity for aldehydes, alcohols and
ketones and they are less responsive to molecules like terpenes, aromatic compounds or organic acids.
To solve the lack of selectivity, some approaches have been undertaken. One option is to increase the
sensitivity and selectivity of the sensor by exploitation of the operating temperatures for the sensor.
Thermal cycling of semi-conductor gas sensors take the advantage of the fact that different classes of
reducing gases have different reaction rates. For example, carbon monoxide and hydrogen sulfide will
oxide on the sensor at relatively low temperatures (starting near room temperature), alcohols and
ketones at intermediate temperatures (200 ºC and above) and alkanes (propane and methane in
particular) at high temperatures (above about 400 ºC). Thus sensors run at different temperatures will
show a degree of selectivity to each gas without increasing the number of sensors [6]. From this point
of view, it has been already shown that, for some applications, a significant improvement in terms of
selectivity can be obtained by selecting an appropriate temperature profile, even though this approach
has not been exploited for food analysis [7-11]. Another novel option to improve selectivity and
independence of sensors is the use of tin dioxide and chromium titanium oxide thick film overlaid with
zeolites [12-15]. Zeolites, microporous and aluminosilicate minerals, are ideal for modifying the
composition of the gas phase within a porous body. They catalyse and they are size- and shape-
specific cracking with partial oxidation.
This review article focuses on the use of MOS-based electronic noses for food applications, the
technical limitations for some applications and the different approaches undertaken to overcome them.
Problems that have been tried to solve with MOS-based electronic noses are those related to quality
control, monitoring process, aging, geographical origin, adulteration, contamination and spoilage
(Table 1).

Table 1. Application of MOS based E-noses in the food industry, sensors used
and performance.
Commodity Test No. of Material Commercial Ref.
MOS (C) or
sensors experimental
(E) E-nose
Meat Freshness and type of meat 4* SnO2 C [19]
Microbiological contamination 7 SnO2 thick film E [20]
Origin of meats 6 SnO2 C [22]
Taints 5 SnO2 E [25]
Fish Freshness 6 SnO2, CTO, WO3 C [27]
6 SnO2, CTO, WO3 C [28]
6 SnO2 E [29]
Milk and Adulteration/ Contamination 10 SnO2 C [32]
dairy 12* SnO2 C** [33]
products Off-flavor n.d. n.d. E [35]
12* SnO2 C** [43]
Sensors 2010, 10 3885

Table 1. Cont.
Milk and Aging/ripening 5 SnO2 thin film E [37,38]
dairy products doped with Pd, Pt,
Os, Ni
18 SnO2, CTO, WO3 C [39]
5 n.d. C** [40]
Cheese type 6 SnO2, CTO, WO3 C [41]
Bacterial strains 12 SnO2, CTO, WO3 C [42]
Origin of caseinates 18 SnO2, CTO, WO3 C [44]
Origin of milk 18 SnO2, CTO, WO3 C [45]
Eggs Freshness 8 n.d. E [46]
4 SnO2 E [47]
12 SnO2 thick film C [49]
Grains Contamination by toxin 6* SnO2 C* [51]
10 SnO2 C [50]
Off-flavors 4* SnO2 E [52]
4* SnO2 E [53]
Fruit Ripening changes 10 SnO2 C [54]
2 SnO2 E [56]
10 SnO2 C [59]
5 SnO2 E [60,61]
12 SnO2, CTO, WO3 C [62]
Varieties 16 SnO2 thin film E [63,64]
doped with Cr, Pt
Microbial contamination 6 n.d. C [55]
Shelf life 18 SnO2, CTO, WO3 C [57]
10 SnO2 C [58]
Olive oil Authenticity 6 SnO2, CTO, WO3 C [66]
Taints 18 SnO2, CTO, WO3 C [68,69]
Alcoholic Denomination of origin 4 WO3 E [84]
beverages and vineyard 16 SnO2 thin film E [85]
discrimination doped with Cr, In
10 SnO2 C [86]
4 SnO2 thin film E [87,88]
doped with Pt, Pd
Aging of wines and beers 16 SnO2 thin film E [72]
doped with Cr, In
20 SnO2 E [89]
12 SnO2, CTO, WO3 C [77]
Sensors 2010, 10 3886

Table 1. Cont.
Alcoholic Classification of drinks 12 SnO2, CTO, WO3 C [78]
beverages 6 SnO2, CTO, WO3 C [90]
6 SnO2 E [73]
6* SnO2 C [71]
18 SnO2, CTO, WO3 C [91]
Off-flavors and aromatic 12 SnO2, CTO, WO3 C [79]
compounds 18 SnO2, CTO, WO3 C [91]
16 SnO2 E [93]
16 SnO2 thin film E [95]
16 SnO2 E [94]
Non Grading 4 SnO2 E [97]
alcoholic 10 SnO2 C [98]
beverages Quality/process control 6 SnO2 E [100]
12 SnO2 E [99]
4 SnO2 thin film E [101]
doped with Au, Pt
5 SnO2 thin film E [102]
doped with Au, Pt,
Pd
6 WO3, SnO2 C [103]
Other food Shelf life of nuts 10 SnO2 C [105]
Shelf life of vegetables 5* n.d. E [104]
Bacterial species classification 6 SnO2, CTO, WO3 C [107]
* Modular sensor consisting of MOS and quartz microbalance (QMB) or metal oxide semi-conductor field-effect
transistor (MOSFET)
** The instrument was commercially available at the time of research publication
n.d. Not disclosed

2. Application of MOS to Food

2.1. Meat

Meat is an ideal growth medium for several groups of pathogenic bacteria. Estimation of meat
safety and quality is usually based on microbial cultures. Bacterial strain identification requires a
number of different growth conditions and biochemical tests with overnight or large incubation periods
and skilled personnel, which means that testing may not be frequently performed. Other methods of
determining meat safety involve quantifying volatile compounds associated with the growth of
microorganisms on meat but these are also time consuming [16-18]. Winquist et al. [19] evaluated
pork and beef freshly ground using ten metal oxide semi-conductor field-effect transistor sensors
(MOSFETs) with thin catalytic active metals like Pt, Ir and Pd, and four SnO2 based Taguchi type
sensors (Figaro Engineering Inc, Japan). Compared to MOS sensors, MOSFETs rely on a change of
electrostatic potential and they are based on the modulation of charge concentration by a MOS
capacitance between a body electrode and a gate electrode located above the body and insulated from
Sensors 2010, 10 3887

all other device regions by a gate dielectric layer which in the case of a MOSFET is an oxide, such as
silicon dioxide [1]. A carbon dioxide detector based on infrared ray absorption (Rieken Keiki Co,
Japan) was also included in the array. The array of sensors was able to determine the type of meat and
predict the storage time as well. When the carbon dioxide monitor was omitted the performance in
predicting storage time decreased. Carbon dioxide concentration is an important parameter to consider
for predicting shelf life storage of meat products. Balasubramanian et al. [20] evaluated the changes in
the headspace of vacuum packaged beef strip loins inoculated with Salmonella typhimurium using a
metal oxide based electronic nose. The E-nose housed seven thick film SnO2 MOS sensors (Figaro
Engineering Inc, Japan). Microbiological measures as a standard method to determine spoilage level
included Salmonella counts and total aerobic counts. The average prediction accuracy of the E-nose
responses was 69.4% using step-wise linear regression principal components (PC) as input. The
accuracy of predicting was improved to 83% when using independent components (IC). PCA is a
second-order linear transformation method of data representation which assumes that data follows a
Gaussian distribution and uses the variance within the data set to estimate the transform. IC analysis is
a relatively new multivariate data analysis that assumes data is non-Gaussian and uses data density
information to estimate the transform [21].
Vernat-Rossi et al. [22] studied the ability of six tin oxide semi-conductors (FOX 2000, France) to
discriminate cured products (dry sausages of various origins or cured hams of different qualities) and
also to determine the presence of pathogenic bacterial strains. Using these sensors it was possible to
classify 98% of the bacterial strains, 94% of the dry sausages and 87% of cured hams into their
respective groups.
Although most applications of metal oxide semi-conductors based sensors in meat have been
focused on rapid methods for detecting spoilage by bacterial contamination, some work has also been
conducted to determine the presence of off-flavors in meat. In many countries pork production from
intact, i.e., non-castrated males, is discouraged because of the unpleasant cooking odor known as “boar
taint”. 5a-Androst-16-en-3-one (5a-An) has been identified as the main compound responsible for the
urine like-odor associated with boar taint [23], with 3-methylindole (“skatole”) and indole, produced
as a result of the metabolism of tryptophan in the intestine, also associated with the taint. There have
also been some efforts to identify the main thermally generated volatile compounds that are related to
the presence of androstenone [24]. Bourrounet et al. [25] used 14 commercially available MOS sensors
to classify fat samples from intact male pigs. Samples were first separated in two classes according to
the levels of androstenone estimated using ELISA assay, <0.7 µg/g and >1.7 µg/g, respectively.
Statistical analysis demonstrated that MOS sensors could classify 84.2% of the samples in two classes.

2.2. Fish

Freshness is the most important factor for fish quality. Traditionally, fish quality evaluation has
been based on organoleptic tests. This type of testing is subjective even when performed by
experienced and well-trained personnel. Gas chromatography has revealed that many volatile
compounds are released from degrading fish, some of which can be used as indicators of spoilage.
Electronic nose are suitable instruments for measuring fish freshness since a large number of volatile
compounds are related to “offness” [26]. Olafsdottir et al. [27] employed six MOS sensors
Sensors 2010, 10 3888

(“FishNose”, AlphaMOS-France) to evaluate cold smoked Atlantic salmon and compared the results
with sensory analysis and microbial counts. In this research salmon were obtained from smokehouses
in Norway, Iceland and Germany and stored in different packing for up to four weeks. Samples were
also submitted to chemical analysis including total fat, salt content, water content and chloride content.
Partial least square regression modeling, with gas sensors as predictors and sensory attributes as
response variables, showed that there is a general correlation between gas sensors and “off-odor” and
“sweet/sour” odor attributes. However, the correlation with the chemical parameters was low which
meant that they could not be used to calibrate the “FishNose”. With respect to microbial analysis, one
sensor type, “PA/2”, showed a very similar pattern to the total viable microbial counts. This work
demonstrated that an E-nose could be used for fast quality control and freshness evaluation of smoked
salmon products related to microbially produced volatile compounds.
The same E-nose was later used to control processing of smoked salmon in a production plant [28].
It was necessary to correct the sensor reading in this case due to the varying ambient air conditions at
the plant. The results showed classification rates ranged between 93% and 95% of fresh samples
whereas, for the aged samples, the rate ranged from 81% to 93%. It was not disclosed if these
percentages are acceptable for quality control purposes or whether the instrument has been adopted for
quality control by the salmon industry.
Sardines have also been the subject of research with the metal oxide semi-conductor sensors. El
Barbri et al. [29] developed a simple electronic nose based on commercially available metal oxide
sensors in order to monitor the freshness of sardines stored at 4 ºC. Principal component analysis
(Figure 1) showed that sardine samples could be grouped according to freshness (“fresh”, “medium”,
“aged”). This classification was directly related to the number of days that sardines were stored. Other
supervised techniques were applied successfully corroborating the usefulness of the sensors to classify
samples. The same authors [30] later incorporated a dedicated real-time data acquisition system based
on a microcontroller and portable computer in order to miniaturize the device.

Figure 1. Scores plot of a PCA on sardine data using the six-element gas sensors array.
A vertical line separating fresh samples from medium and aged ones and ellipses grouping
fresh, medium and aged samples had been added for easy identification (reprinted from
[29] with permission from Elsevier, copyright 2007).
Sensors 2010, 10 3889

2.3. Milk and Dairy Products

It is in the area of milk and other dairy products that there has been extensive research in evaluating
electronic noses for monitoring the quality of these products. Areas of research have ranged from
detecting adulteration/contamination of milk to determining the geographical origins of cheese. A list
of reported applications is given below.

2.3.1. Adulteration/ contamination of milk and off-flavors

Liquid milk is an essential nutritional food for infants. Adulteration of milk with water is a matter
of serious concern because of the lower nutritional value provided to consumers. The dairy industry
employs various quality checks which include the determination of fat and total solids by chemical or
physical analyses; estimation of sediment; determination of bacterial count, determination of freezing
point, protein, etc. [31]. However, most of these measurements are expensive and time consuming
since milk samples need to be taken to a laboratory for testing. Yu et al. [32] monitored the
adulteration of milk using an E-nose (PEN2, Germany) containing ten different metal oxide semi-
conductor sensors. Whole milk, reconstituted milk powder and whole milk adulterated with different
proportions of water or reconstituted milk powder were followed in storage for 7 days at 20 ºC. In this
study, the E-nose was able to discriminate skim milk adulterated with different volumes of water and
reconstituted milk, and also able to discriminate 100% skim milk samples between 1 and 4 days of
storage. However it was not able to discriminate samples between 5 and 7 days of shelf life.
Another area related to milk quality and safety is the detection of contaminants, including
aflatoxins, in milk. Benedetti et al. [33] studied the feasibility of using a commercial sensor array
system, comprising 12 MOS and 12 MOSFET sensors, to detect the presence of aflatoxin M1 (AFM1).
The E-nose classification was in complete agreement with aflatoxin M1 content measured by an
ELISA procedure. An additional advantage of this approach is that it can be applied to rapid screening
for AFM1 contamination in random samples taken at various places through a lot or sub-lot. Samples
which are identified as contaminated in the screening process can then be sent for further
characterization using quantitative analytical methods, or else rejected to avoid contamination of the
entire lot [33]. Factors which are known to the development of oxidized off-flavor in milk products
include the contamination of milk with copper, iron, rust and chlorine, or exposure to sunlight as well
as excessive incorporation of air. Other off-flavors in milk may be derived from excessive heating
which can especially cause certain proteins (such as whey proteins) to burn. Whey proteins are a rich
source of sulfide bonds which can form sulfhydryl compounds which can then contribute to off-flavor
[34]. Great efforts have been devoted to the optimization of ultra high temperature (UHT) milk
processing in order to avoid this effect. One study using an E-nose comprising of MOSFET, MOS and
quartz microbalance (QMB) sensors found that it could discriminate as little as 10% boiled milk in
pure UHT milk whereas a sensory panel, in contrast, could not discriminate proportions of UHT below
30% [35]. QMB are sensors made of tiny discs, usually quartz, coated with materials such as
chromatographic stationary phases that are chemically and thermally stable. When an alternating
electrical potential is applied at room temperature, the crystal vibrates at a very stable frequency,
defined by its mechanical properties. Upon exposure to a vapor, the coating adsorbs certain molecules
Sensors 2010, 10 3890

which increases the mass of the sensing layer and hence, decreases the resonance frequency of the
crystal.

2.3.2. Ageing of milk

One of most important steps in manufacturing dairy products is the quality control of the starting
material. Chemical analysis of flavors in dairy products is often complicated due to the heterogeneous
nature of milk. High concentrations of lipids, proteins and carbohydrates in milk can make it difficult
to separate flavor-active chemicals based on general properties like polarity or volatility. Furthermore,
the headspace of milk typically represents a complex mixture of organic volatiles at varying
concentrations and at high relative humidity. Profiling the volatile components in milk and dairy
products is usually performed by dynamic or static headspace, “purge and trap” techniques, etc with
measurement by gas chromatography-mass spectrometry (GC-MS) [36]. E-noses can also detect milk
volatile compounds and are able to monitor the aging of milk [37,38]. An E-nose with five different
SnO2 thin films, prepared using sol-gel technology, was used to measure the development of rancidity
in UHT and pasteurized milk during 8 and 3 days, respectively. The sensors could distinguish between
both types of milk as well as determine the degree of rancidity of milks (Figure 2). Labreche et al. [39]
obtained similar results with an E-nose housing 18 MOS sensors (FOX 4000, France). The E-nose
detected significant changes in headspace during milk aging. The authors claimed that there was a high
correlation between bacterial counts and the sensor responses.

Figure 2. PCA plot based on E-nose measurements of (a) UHT milk and (b) pasteurized
milk showing ageing of milk over 8 and 3 days respectively (reprinted from [37] with
permission from Elsevier, copyright (2001).
a b

2.3.3. Ripening of cheese and cheese types

The ripening of Swiss Emmental cheese has been followed with several instruments such as QMB,
conductive polymer (CP), mass spectrometer system (MS), MOSFET and a set of MOS [40]. On their
own, QMB sensors were not able to discriminate between cheeses ripened between day 1 and 180
Sensors 2010, 10 3891

days, and the MS was not sensitive enough to detect differences among the samples while the
MOSFET was not able to provide good discrimination. However, when the MOSFET was combined
with MOS, a good correlation was found with the cheese ripening. Overall, MOS were the most
efficient sensors for discriminating among the four stages of ripening. This study also used an unusual
system, “trapped flow”, for presenting samples to the E-nose. With trapped flow, the headspace
compounds are retained in the sensor chamber for a certain amount of time which allows a better
interaction with sensor coatings and consequently stronger responses. However this approach also
causes more wear on the sensors. Within less than one year, four of the MOS sensors had to be
replaced. The damage was probably caused by the high levels of free fatty acids present in this cheese
type and released into the headspace. It was believed that the weak acids react irreversibly with sensor
coatings, leading to their accelerated aging. Other workers [41] have used six MOS sensors (FOX
2000, France) to evaluate Swiss type cheeses labeled with different flavors as 0% fat, 33% reduced-fat,
sharp, bland and a Norwegian Jarlsburg cheese. The E-nose was able to correctly classify cheeses and
it was in agreement with solid phase microextraction-gas chromatography with flame ionization
detector (SPME-GC-FID) analysis and sensory analysis.

2.3.4. Lactic acid bacteria

There is a strong interest in exploring the potential of novel Lactococcus lactis strains isolated from
Nature for the production of aroma in cheeses and other dairy products [42]. A MOS-based electronic
nose (FOX 3000, France) with sensory evaluation have been used to evaluate their potential to screen
the aroma generation of Lactococcus lactis strains as cheese starter cultures [42]. Twenty-three strains
of Lactococcus lactis were isolated from dairy sources such as boutique raw-milk cheeses, non-dairy
sources, and commercial starter cultures (industrial). PCA based on E-nose data revealed four
distinctive groups based on aroma profiles that were not correlated with their origin, which also agreed
with the results of the sensory analysis.

2.3.5. Off-flavors in cheese

Emmental cheese can develop a “rind taste” off-flavor that can be identified by tasting the cheese at
the hoop side (curved side). The components responsible for this off-flavor are often not eliminated
during manufacturing, and so may therefore be present in the final product. Cheese loaves must
therefore be treated carefully during ripening in order to avoid this problem. The cut pieces are either
used fresh or stored in a freezer room which slows down the oxidation process. Attempts to identify
the volatile basis of “rind taste” using GC-MS have been unsuccessful [43]. Tainted and untainted
Emmental cheeses gave the same profile with the only differences seen being those due to the stage of
maturity. A MOS based-E-nose was also totally unable to discriminate contaminated from non
contaminated samples. These workers [43] concluded that the rind-related compounds were either not
volatiles compounds or were present at levels below the detection threshold of these instruments.
Sensors 2010, 10 3892

2.3.6. Geographical origin of dairy product

A study on the discrimination of caseinates from different origins was conducted with an E-nose
(FOX 4000, France) [44]. PCA and discriminant canonical analysis (DCA) were able to distinguish
and classify all samples correctly. The results were validated with measurements of unknown samples
obtained from a different supplier and the E-nose showed to be efficient to discriminate the quality
between the different suppliers. Similarly, milks from different origins (different brands) that had been
pasteurized using similar process were easily distinguished by the same E-nose [45].

2.4. Eggs

One of the main concerns of the egg industry is the systematic determination of egg freshness,
because some consumers perceive variability in freshness as lack of quality [46]. The modern poultry
industry is not satisfied with the traditional system for the handling and processing of eggs, which is
based on visual inspection of eggs, mainly because it is time consuming and is not error-free. The
industry is therefore interested in evaluating alternative ways that can be used to measure quality
parameters more quickly. The main quality parameters of interest are: freshness, weight and shape,
state of the eggshell, size of air cell, albumen and yolk quality, the ratio of albumen weight to egg
weight (Haugh unit) and eggshell thickness [47]. An alternative strategy for determining the state of
freshness of eggs is to detect the organic volatiles emitted by eggs with an E-nose. Methyl sulfide-
compounds are good candidates for freshness determination because they are directly related to
deterioration and perception of unacceptable odors in whole eggs [48]. Dutta et al. [47] used four tin-
oxide odor sensors (Figaro Engineering Inc, Japan) to classify eggs non-destructively. Three different
freshness categories were identified using PCA which was in good agreement with the three categories
of egg freshness determined from the ‘use by date’ of the egg samples. Ninety-five percent
classification accuracy was achieved using a radial basis function network.
Suman et al. [49] compared the performance of an E-nose based on metal oxide semi-conductors
with classical chemical and sensory methods for quality control of manufactured egg products. A
trained sensory panel evaluated egg samples against the descriptors ‘strong egg odor’, ‘slightly
pungent’ and ‘pungent’. Lactic acid and succinic acid in the egg products were determined
enzymatically while microbiological analyses included total viable mesophilic bacteria and
Enterobacteriaceae counts. The researchers employed a destructive method to evaluate freshness of
eggs with E-nose where fresh egg products were spiked and homogenized with different percentages
of degraded eggs to obtain different degradation levels. The E-nose demonstrated a high degree of
discrimination of samples analyzed during their degradation process compared to chemical and
microbiological tests. Wang et al. [46] developed prediction models for egg internal quality using an
E-nose signal. The E-nose was able to distinguish different storage times under cool (4 ºC) and room
temperature conditions (21 ºC). Moreover, prediction models of the main indicators of internal quality
of eggs i.e., Haugh unit and yolk factor (ratio of yolk height and width), using E-nose responses
indicated a good prediction performance (Figure 3). Haugh unit had a standard error of prediction
(SEP) of 3.74 and a correlation coefficient of 0.91; the yolk factor model had a SEP = 0.02 and
correlation coefficient of 0.93 between predicted and measured values respectively.
Sensors 2010, 10 3893

Figure 3. Predicted versus E-nose-measured values of egg quality indices from quadratic
polynomial step regression models (a) Haugh unit and (b) yolk factor (reprinted from [46]
with permission from Elsevier, copyright 2009).

2.5. Grains

Aflatoxins and deoxynivalenol (DON) are highly toxic and carcinogenic secondary metabolites
produced by fungi, mainly the genus Aspergillus and Fusarium. These toxins are found regularly in
food commodities, including cereals for human and animal consumption. Warm and/or humid storage
conditions for cereals can result in the growth of toxigenic fungi and synthesis of metabolites including
dangerous mycotoxins [50]. Because of the highly heterogeneous distribution of mycotoxins in
contaminated food supplies, there is a need for cost-effective analytical methods that can process
multiple samples from the same lot. Headspace analysis using sensor array appears to be a promising
solution. Campagnoli et al. [50] employed a commercially available E-nose with ten metal oxide
semi-conductor sensors to discriminate between mycotoxin contaminated and un-contaminated cereals.
Two of the sensors had partial correlations with the level of aflatoxins in maize. Other two sensors
showed high sensitivity towards wheat samples with DON. In both cases 100% correct classification
was obtained using linear discriminant analysis (LDA). In another research work, Olsson et al. [51]
demonstrated that GC-MS system predicted ochratoxin OA concentrations in barley grains with a
higher accuracy than ten MOSFET sensor and six SnO2 Taguchi sensors, since the GC-MS
misclassified only 3 of 37 samples and the electronic nose 7 of 37.
Other applications of E-nose to grains include measuring off-odors indicative of past or ongoing
microbial deterioration [52,53]. Borjesson et al. [52] tried to classify samples of wheat, barley and oats
based on sensory attributes ‘moldy/musty’, ‘acid/sour’, ‘burnt’ and ‘normal’. These workers used ten
metal oxide semi-conductor field effect transistor (MOSFET) sensors and four different SnO2
semi-conductors. Prediction of the degree of ‘mold/musty’ odor was also included in the study. The
E-nose correctly classified 75% of samples according to the four descriptors. Ninety percent of the
samples could be correctly assigned using a two-class system ‘good’ and ‘bad’. These values exceed
the levels of agreement between two human grain inspectors classifying the same samples.
Jonsson at al. [53] confirmed these results using the same set of sensors. Sensors could predict the
following odor attributes: ‘good’, ‘moldy’, ‘weak musty’ and ‘strong musty’ in oats with high
accuracy (100% good prediction). In wheat, correlations of 0.99, 0.84 and 0.88 were found between
Sensors 2010, 10 3894

measured and predicted levels of fungal colony-forming unit (cfu), bacterial cfu and ergosterol in
µg g−1, respectively.

2.6. Fruits

The aroma of fruits and vegetables are either formed during ripening or upon tissue disruption,
which occurs after maceration, blending or homogenization. Many volatile compounds are naturally
formed by enzymes found in the intact tissue of fruits and vegetables. They originate from secondary
metabolites with various biosynthetic pathways. The characteristic aroma of fruits is an important
factor in their overall acceptance by the consumer. For many years human senses have been the
primary “instrument” that has been used to determine fruit quality. More recently, techniques such as
gas chromatography-mass spectrometry (GC-MS) have been used to characterize the volatile profiles
of fruits and vegetables. However, it is neither feasible nor practical to use techniques such as GC-MS
or sensory panel to assess cultivars or product found at storage stations. Consequently, E-noses have
the potential to fill this gap since they are a rapid, transportable and an objective measurement tool for
aroma analysis. Gomez et al. [54] evaluated the capacity of ten metal oxide semi-conductor sensors
(PEN2, Germany) to monitor the change in volatile production during tomato ripening. The E-nose
was able to discriminate among different ripeness stages (“unripe”, “half-ripe”, “fully-ripe” and “over-
ripe”) with LDA showing 100% correct classification of samples. In the same way, an EOS835 E-nose
with six thin film MOS sensors was tested for its ability to determine microbial contamination in
canned peeled tomatoes [55]. Tomatoes were artificially contaminated with different microbial flora
and analyzed by electronic nose, and the E-nose was able to detect contamination at early stages
depending on the type of contamination (e.g. Saccharomyces cerevisiae and Escherichia coli) as well
as classify spoiled tomato samples with high fidelity.
Other fruits including blueberries, melons, snake fruit and mandarins have been evaluated by
MOS-based electronic noses either to predict the optimal harvest day (OHD) or to monitor shelf life.
Blueberry is a highly perishable fruit that must be processed properly and with care otherwise it can
develop damage such as cracks, leaks, soft spoilage, which will be apparent to the consumer. Simon et
al. [56] were able to detect 5% soft and damaged blueberry fruit in packaged containers with just two
tin oxide gas sensors and could also distinguish four of five fruit ripeness classes. The sensor responses
correlated well with other quality indicators like berry firmness, pH titratable acidity, and color. These
workers also detected differences among ten cultivars. In a similar study on snake fruit, three out
of 18 MOS-based E-nose (FOX 4000, France) were found able to discriminate among maturity
levels [57]. For mandarins however, a sensor array of ten different metal oxide semi-conductor sensors
(PEN2, Germany) was not effective in separating mandarins based on different storage times [58]. In
contrast, though the same E-nose could detect differences in mandarins picked on different dates and
also evaluate mandarin quality attributes such as firmness, soluble solids content and acidity [59]. In a
different study with melons and using another E-nose, MOS sensor responses were found to be highly
correlated with the sugar content of melon samples harvested at different stages, demonstrating that it
could be used to predict the OHD [60,61]. OHD is also of importance in those fruits which are used for
further processing, like winegrapes. Berna et al. [62] suggested that a MOS based-E-nose (FOX 3000,
France) may be a useful practical tool to estimate the time to ripeness of grapes. Preliminary results
Sensors 2010, 10 3895

demonstrated that the E-nose can predict the geographical origins of winegrape samples from five
South Australian valleys. LDA of the E-nose responses showed that 87% for both Cabernet Sauvignon
and Riesling juice were correctly classified [62]. Likewise, an E-nose based on 12 MOS sensors was
successful in distinguishing among Spanish wine grape juice varieties, and between red and white
wine grape juices [63,64].

2.7. Olive Oils

Virgin olive oils (VOO), and in particular, extra-virgin olive oils (EVOO), are produced using cold
pressing techniques. They are sought-after olive oil product because of their aroma, taste, antioxidant,
and nutritional properties. The cultivation of olive trees, harvesting of the fruit, and extraction of olive
oil are labor intensive and time consuming tasks which add considerably to the overall cost of the oil.
Attempts to adulterate VOO with less expensive vegetable oils or lower quality olive oils are thus by
no means rare. Not only does this practice defraud consumers, but also constitutes a threat to the
reputation and economic development of Mediterranean agricultural communities [65]. Aroma is a
fundamental component of the sensory quality of olive oils but sensory panels cannot be used to assess
the aroma due to the large number of samples that need to be screened. Gonzales et al. [66] used an
array of metal oxide semi-conductor gas sensors (FOX 3000, France) to discriminate VOO from
non-VOO. The test set comprised 141 commercially available oils of various origins and from
different suppliers. Of these samples around 29% were labeled as VOO. Linear discriminant analysis
(LDA) applied to the responses of the MOS sensors was able to classify olive oils with 95% of
accuracy, indicating that the sensors could determine adulteration of olive oil products.
Other common problems in olive oils are defects caused by chemical taints, mainly volatiles. These
may be formed from a number of sources. These include oxidation of unsaturated fatty acids, overripe
fruit, molds or bacterial contamination. Trained panels are commonly used to evaluate these defects.
Indeed, regulators in the European Union and the International Olive Oil Council (IOOC) [67] have
adopted a common standard for assessment of VOOs. The sensory characters of VOO are classified by
the IOOC into positive and negative attributes. Negative attributes included: “fusty”, “musty”, “muddy
sediment”, “vinegary”, “metallic” and “rancid”. Garcia-Gonzalez et al. [68] studied the detection of
“vinegary” attribute, produced by acetic bacteria which grow during the storage of olives, using an 18
MOS (FOX 4000, France); six of these sensors were undoped and the remainder doped with metals to
shift their selectivity spectrum. The array was trained on a set of Spanish VOOs spiked with different
concentrations of acetic acid while the test set comprised Italian VOOs spiked with a standard
vinegary VOO supplied by the IOOC. For both varietal VOOs, there was a good linear relationship
between levels of acetic acid and the sensor responses (R2 = 0.97 and 0.98 for Spanish and Italian
VOO, respectively). The same E-nose was evaluated for its capacity to detect other attributes in olive
oils like “rancid” and “fusty” [69]. In this case degraded samples were prepared by placing VOO
samples under ultraviolet light for up to 12 days or by the addition of different concentrations of a
“fusty” standard supplied by IOOC. Correlations of 0.91 for the “fusty” and 0.85 for the “rancid”
attribute were found between E-nose sensor responses and sensory evaluations. Using LDA with
sensor responses, it was possible to classify defective samples. Samples characterized by the vinegar
Sensors 2010, 10 3896

attribute were clearly distinguished from rancid and fusty samples, a small overlap was observed
between fusty and rancid defective samples. The percentage of misclassification was not disclosed.

2.8. Alcoholic Drinks

While metal oxide semi-conductors are probably the most widely used of the E-nose sensors, they
have still some significant limitations when applied to alcoholic drinks. MOS responses depend
logarithmically on the concentration of analyte gases. In the presence of very high concentrations of
analyte, such as ethanol in alcoholic beverages, sensors become saturated and mask the responses to
other volatile compounds. Consequently, samples tend to be differentiated on the basis of variations in
ethanol content rather than the other volatile compounds which are responsible for the aroma [70].
Several strategies have been developed to decrease ethanol content and increase concentration of other
volatile compounds before E-nose analysis. These include: the use of a chromatographic column
between the headspace sampler and the sensor array to eliminate ethanol [71], and a purge and trap
step to eliminate water and ethanol [72]. Other techniques include solid phase micro-extraction
(SPME) [73], pervaporation [74,75] or dynamic headspace sampling using resin [76]. Other
researchers have successfully dried wine samples on nylon membranes prior to E-nose analysis
[77-80]. Beer samples pose an additional problem due to the super-saturation of CO2 and foam
formation when the samples are heated for headspace sampling. Different approaches have been tested
to liberate CO2 such as NaCl addition at low temperature [81], nitrogen sparging [82] or simple
agitation [83]. Notwithstanding the special challenges presented by alcoholic beverages, E-noses have
been used widely to analyze alcoholic beverages, as described below.

2.8.1. Discrimination of wines by denomination of origin and vineyard

Discrimination of wines is not an easy task due to the complexity and heterogeneity of the
headspace. However, classification of wines is an economically important application because of high
value of wines from specific geographical regions and also the need to prevent illegal substitution or
adulteration. Current methods to evaluate wines include sensory analysis but, because of its high cost,
E-noses have been evaluated as an alternative. Penza et al. [84] tested three red, three white and three
rosé wines from different Italian denominations of origin and vintages using a multisensor array that
incorporated four metal oxide (WO3) semi-conductor thin film sensors. Static headspace sampling
(SHS) was used to sample the volatile compounds above the wine sample. Although SHS, as
recognized by the authors [84], is very sensitive to volatile compounds like ethanol and scarcely able
to detect trace compounds, it is also a simple, fast and reproducible sampling method that can be used
with an automated extraction process. Furthermore it is also low-cost and a solvent free method.
Neural network classification of the E-nose data correctly predicted 100% of the white wines, 77.8%
of the red wines but only 33.3% of rosé wines. Other researchers [85] employed SHS followed by
dynamic headspace to classify Spanish wines according to their geographic origin. Multivariate
statistical analysis showed that all the tested wines were different. Buratti et al. [86] employed ten
metal oxide semi-conductors type chemical sensor (PEN2, Germany) and an enrichment desorption
unit to trap and thermally desorb wine samples into the E-nose. The sorbent material was Tenax®-TA
Sensors 2010, 10 3897

polymer and the wine samples came from two northern Italian regions. LDA applied to a larger data
set (i.e., chemical analysis, E-nose, Etongue and color measurements) correctly classified 100% of
wines into their region. The error rate using only E-nose responses was not disclosed. Berna et al. [80]
compared E-nose (12 MOS sensors, FOX 3000) SPME measurements after drying wine samples on a
nylon membrane with SHS for predicting the regional origins of 34 Sauvignon Blanc wines. GC-MS
was also used to analyze all wine samples. LDA applied to GC-MS data showed that there were three
distinct clusters or classes of wines with different aroma profiles (Figure 4). After training the E-nose
based on GC-MS grouping of wines, the average error of prediction was 6.5% with SPME compared
with 24% using SHS.
Di Natale et al. [87, 88] employed four MOS sensors to classify wines having the same geographic
origin but coming from different vineyards. The E-nose was found superior to the standard chemical
analysis routinely executed by the wineries. The standard analysis failed to distinguish classes mainly
characterized by the same amount of free SO2.

Figure 4. Score plot of the first two canonical variables of the linear discriminate analysis
based on the intensity of mass to charge ratio of 34 wines. The symbols represent the six
geographical origins of Sauvignon Blanc wines samples. Loire (♦), Marlborough (▲),
South Australia (∆), Tasmania (●), Victoria (+), Western Australia (○) (reprinted from [80]
with permission from Elsevier, copyright 2009).

2.8.2. Aging of wines and beers

Aging of wines and beers allows desirable flavors and aromas to develop and off-flavor notes to
diminish. Volatile chemicals are an important component of wine and beer flavor and it is desirable to
monitor them through aging. Garcia et al. [72] analyzed wines of the same variety and geographical
origin that differed in age after fermentation (young wines, aged for a year, aged for 18 months and
aged for 24 months). They compared two sampling systems, SHS and dynamic headspace with purge
and trap, with a 16 MOS sensor array. With SHS sampling 80% of the wines were correctly classified
while with purge and trap, a technique more efficient in decreasing moisture and ethanol content in the
Sensors 2010, 10 3898

headspace, the success rate was 95%. More recently, Villanueva et al. [89] used 20 MOS sensors
combined with SPME to discriminate wines aged for 3 and 6 months in oak barrels. The E-nose clearly
distinguished between aging times and was in good agreement with chemical analysis and sensory
panel evaluations. McKellar et al. [77] attempted to determine the influence of aging time on the
development of aroma characteristics of a commercial beer (“Sleeman Cream Ale”) with an E-nose
(FOX 3000, France). SHS was the sampling method of choice. The E-nose was able to separate beer
samples into distinct groups with those aged up to 12 or 14 days separated from samples aged longer
than 14 days. These findings were confirmed by GC-MS. Aging beer for longer than 5 to 7 days
appears to have no significant advantage in removing fermentation odors. The authors concluded that
reducing the time required in the aging tank would reduce costs to the brewer.

2.8.3. Classification of alcoholic drinks

McKellar et al. [78] used a MOS based-E-nose (FOX 3000, France) for the classification of eight
fruit wines (blueberry, cherry, raspberry, blackcurrant, elderberry, cranberry, apple and peach) and
four grape wines (red, Chardonnay, Riesling and ice wine), and each variety of wine obtained from a
minimum of five Ontario wineries. The wine samples were dried onto membrane filters to remove
ethanol. Each of the 12 different wine varieties could be separated according to winery. The E-nose
appeared to be distinguishing volatile patterns that were characteristic of each winery or the
wine-making procedure. However, the E-nose was less able to separate the 12 varieties of wines from
each other, in part owing to the variation among wineries. Although the E-nose failed to find
dissimilarities between fruit wines, the same type of E-nose (FOX 2000, France) seems to be more
efficient to discriminate between other alcoholic beverages like tequila, whisky, vodka, wine and beer
as found by Ragazzo-Sanchez et al. [90]. The authors used gas chromatogram (GC) to remove ethanol
and dehydrate headspace beverages with the remaining volatile compounds collected by reverting the
gas using column ‘back-flush’ and introduced in the injector port of the E-nose. PCA analysis showed
that most beverages were correctly discriminated, except for some confusion between tequilas and
whiskies. Interestingly, the order of the classification along the PC axis was not related to the initial
ethanol content. Aishima et al. [73] succeeded in classifying eight liquors (shochu, white and red
wines, beer, sake, whiskies and cognac) with six semi-conductor gas sensors. In this case volatiles
were pre-concentrated in a Tenax®-TA trap to remove ethanol. Others [71], using chromatographic
preseparation, have characterized the ‘flavor peaks’ of different beer brands using a modular sensor
array set up consisting of eight quartz microbalance (QMB) and eight SnO2 based MOS sensors
(MOSES II, Germany). Without the removal of the ethanol content (similar in each sample), it was
impossible to discriminate beer brands (Figure 5a). However after pre-separation, beer brands could be
perfectly distinguished (Figure 5b). Similar results were found by Ragazzo-Sanchez et al. [91]
using 18 MOS E-nose (FOX 4000, France) and sample agitation to reduce CO2 from headspace. The
E-nose successfully discriminated three classes of beers even though the beer samples were spiked
with off-flavors.
Sensors 2010, 10 3899

Figure 5. Score plot of eight different beer brands measured with a MOSES II E-nose
(a) without pre-separation unit and (b) with pre-separation unit consisted of thermostated
gas chromatography column installed between the headspace sampler and the sensor array
(reprinted from [71] with permission from Elsevier, copyright 2000).

2.8.4. Detection of aromatic compounds and off-favors in wines

A wine fault or defect is an unpleasant characteristic of a wine often resulting from failures in
winemaking or storage conditions. Normally, many of the compounds that cause wine faults are
present in wine at concentrations which do not adversely affect it. However when these concentrations
exceed the sensory threshold, the resulting aroma can overwhelm or obscure the desirable flavors and
aromas of the wine. The quality of the wine is reduced, making it less appealing and sometimes
undrinkable. Some of the most common off-flavor metabolites are produced by Brettanomyces yeasts:
4-ethylphenol (4EP) and 4-ethylguaiacol (4EG). Typically these taints are described as “barnyard”,
Sensors 2010, 10 3900

“sweaty saddle” and “band-aid” when present in red wine at concentrations of several hundred µg L–1
or more. Using nylon membranes to remove ethanol, Berna et al. [79] established that the detection
limits for a MOS-E-nose (FOX 3000, France) were 44 µg L–1 for 4EP and 91 µg L–1 for 4EG
(Table 2); these values are significantly lower than the reported human sensory thresholds of 605 and
110 µg L–1 for 4EP and 4EG, respectively [92]. Partial least squares (PLS) regression of electronic
nose signals against the known levels of 4EP and 4EG in 46 Australian red wines showed that the
MOS-E-nose was unable to identify Brettanomyces spoilage reliably due to the gas sensors responding
to inter-sample variation in volatile compounds in the samples rather than the ethylphenol content. It
was concluded that, following ethanol removal, existing metal oxide sensors are sufficiently sensitive
to detect Brett taints in wine but lack the selectivity needed to perform this task when the aroma
volatiles background varies. This lack of selectivity was confirmed later by Ragazzo et al. [91] who
attempted to predict the presence of off-flavors like, ethyl acetate (“oxide” attribute),
2,4,6-trichloroanisole (“musty/cork” attribute), 4EP (“barnyard” notes) and hexanol (“herbaceous”
attribute), in wines using 18 MOS sensors (FOX 4000, France). If the origin of the wine was known
the prediction error of contaminated wines was 11% however, if the wine was of unknown origin the
E-nose failed to detect the off-flavor. In another work, a 16 MOS based E-nose could discriminate
different aromas spiked in a base white wine with an accuracy of 97.2% [93]. Others found that, when
comparing sensory human panel thresholds with chemical MOS sensors to detect wine-related aroma
compounds, the perception level of the human nose was superior to the E-nose [94,95], but the E-nose
had a better recognition threshold in recognizing a specific odor [94].

Table 2. Equations of the Linear Regression for the Different Compounds with Correlation
Coefficient r2 and detection limit of the linear range (reprinted with permission from [79];
copyright 2008 American Chemical Society).

Linear regression: Detection

E-nose sensor
Compound a×conc. + b limit
type
a b r2 (μg L−1)
4-Ethylphenol SY/G 6.80E-3 –1.02 0.99 101.2
SY/Gh 6.05E-3 –1.13 0.99 138.4
SY/gCT 6.08E-3 –1.34 0.99 43.8
4-Ethylguaiacol SY/Gh 6.75E-4 –0.59 0.81 93.5
SY/gCT 6.60E-4 –0.37 0.78 91.1

2.9. Non-Alcoholic Beverages

Tea and coffee are the most popular beverages which have been the subject to research using
electronic noses, particularly in the evaluation of the quality grades of these products. Because of the
complexity of the organic compounds present in both raw materials, E-noses are suitable for
continuous real time monitoring of odor. Tea grade is traditionally classified by a trained human panel.
In total, 24 non-overlapping flavor terms have been identified out of 40 generally used flavor notes
[96]. Dutta et al. [97] assessed an E-nose for its suitability in monitoring the quality of five Assam tea
samples manufactured under different processing conditions in India. Tea sample variations were
Sensors 2010, 10 3901

based on drying of the product, fermentation and the final oven fired process. Four tin oxide sensors
(Figaro Eng. Inc, Japan) were used to evaluate headspace of liquid tea samples. MOS sensors were
able to discriminate five different categories of tea, indicating that the instrument was able to
discriminate between flavors of teas manufactured under different processing conditions. A
probabilistic neural network used with the E-nose responses provided 100% accuracy in classification
of the tea samples. Yu et al. [98] studied the applicability of an electronic nose for assessing the same
category of tea with different quality grades. Tea samples had five grades (different prices) picked
from the same area and prepared as tea leaf or tea beverage or tea remains. The E-nose housed ten
different metal oxide semi-conductor sensors (PEN2, Airsense Analytics) and LDA of the sensor
responses showed correct classification ratios of 93.3 % and 100% for tea leaf and tea beverage
samples respectively. For tea remains the classification results were not disclosed but appeared to be
not as good as the other two samples.
Like tea, coffee quality is assessed by coffee tasters, largely on the basis of its aroma and flavor.
The highest quality beans command a considerable premium when the product is sold. Coffee volatiles
are numerous and varied in their aroma quality, potency and concentration. Most of the volatiles are
derived from non-volatile components of the raw bean, and formed during roasting to generate a
complex aroma mixture. Green coffee beans are generally regarded as having no agreeable aroma or
flavor but do possess a large number of volatiles, most of which increase in concentration during
coffee roasting even though there is a minority which tend to degrade [99]. Aishima et al. [100]
focused on the ability of six MOS sensors to discriminate coffee beans and instant coffee. They found,
after cluster analysis applied to the normalized responses, a clear separation between coffee beans and
instant coffees. Stepwise LDA applied to the data matrix showed that a single sensor (TGS812) could
effectively discriminate coffee aromas. On its own that sensor correctly classified 78% of samples.
When four sensors were included in the model the classification could perfectly discriminate among
two ground coffees and two instant coffees. Correlation coefficients between sensor responses ranged
between 0.90 and 0.99 explaining the cross sensitivity of the sensors. Gardner et al. [99] employed an
array of 12 tin oxide sensors to evaluate three commercial coffees (covering two different blends and
two roasted varieties) as well as one coffee sample which was subjected to a range of six roasting
times. For the three commercial coffees, a success rate of 89.9% was achieved when using the entire
data set but this value decreased to 81.1% when half of the data set was used for cross-validation. The
success in predicting roasting time was 88.1%. It seemed that tin oxide gas sensors were suitable for
discriminating between both the blend and roasting level of coffee, confirming the potential of E-noses
for on-line quantitative process control in the coffee industry.
Other application of E-noses to coffees include the study of Pardo et al. [101] who evaluated a
system consisting of four SnO2 thin film sensors, of which two were pure SnO2, another doped with
gold and the last one doped with platinum, to distinguish between commercial coffee blends. Twelve
types of coffees were evaluated in the form of espresso extract and each were sampled at three points
in preparation: as beans, ground powder and liquid. Only two sensors were needed to correctly
classify 100% of the bean samples. In the case of ground coffee, a supervised drift compensation
algorithm was developed and 87.5% correct classification was achieved. On the other hand, liquid
coffee samples were not successfully classified; which the authors attribute to the difficulty in assuring
reproducible sampling conditions. In later work Pardo et al. [102] used the same system with an extra
Sensors 2010, 10 3902

SnO2 sensor doped with palladium in order to evaluate two groups of coffees. The first group
comprised six single coffee varieties and an Italian certified espresso blend while the second group of
coffees consisted of seven blends. The E-nose results were then compared with sensory analysis of the
final product; i.e., cups of espresso, with the panel judging ten quantitative descriptors and four
qualitative descriptors. Using PCA and multilayer perceptrons, 82% of the samples were correctly
classified for the first group of coffee while for the second group, the classification rate was 87%.
Moreover, MOS sensor responses were used to predict single quantitative descriptors and the best
predicted descriptors were “global negative odor” and “global positive odor”, with correlation
coefficients of 0.90 and 0.89, respectively.
Falasconi et al. [103] used a novel Electronic Olfactory System EOS835 (Sacmi Imola, Italy),
housing six thin-film semi-conductor MOS, to monitor the ripening or seasoning process of
commercial coffee blends, made from 12 different types of monocultivar Arabica coffee. Although the
authors focused on the investigation of sampling conditions and feature selection for improving
classification performance, the results showed that EOS835 was suitable to monitor coffee blends
during the seasoning process. Only two sensors performed adequately for this application.

2.10. Other Food

Electronic noses have also been evaluated for their ability to measure shelf life of products like nuts
and fresh cut vegetables [104,105]. Because they have high fat content and therefore are susceptible to
rancidity arising from lipid oxidation nuts are a good model product for shelf life studies [106].
Storage variables such as light and temperature can influence the development of off-flavors. Hexanal
is the main aldehyde formed during oxidation of unsaturated fats and therefore is a good representative
marker of oxidative rancidity [10]. An electronic nose with ten metal oxide semi-conductor sensors
(PEN2, Germany) was compared with GC-MS for the estimation of hexanal formed in hazelnuts
during storage under different conditions (room temperature, 40 ºC, ultraviolet light, with and without
oxygen scavenger) [105]. The results obtained with the two instruments correlated well. The E-nose
discriminated nut samples stored under UV light without oxygen scavenger from the rest of samples.
Differences were not observed between samples stored at 40 ºC and at room temperature. Metal oxide
semi-conductors based E-noses have also been used to shelf life studies of fresh cut vegetables [104].
Minimally processed vegetables (MPV) are fresh raw vegetables that are sold ready-to-use. They are
usually peeled, washed, dried and are sometimes cut and packaged in either sealed pouches or wrapped
trays. The degradation of MPV is a complex process which includes microbial spoilage and a number
of physico-chemical and bio-chemical modifications that mainly affect the sensory properties of the
product. Spoilage may be detected through the analysis of off-odors produced by bacteria.
Riva et al. [104] used an E-nose equipped with ten MOSFET and five MOS sensors to evaluate shelf
life of ready-to-use fresh cut chicory (Cichorium intybus) and carrots (Daucus carota). PCA of the
data demonstrated that E-nose responses correlated well with classical evaluation of vegetable
spoilage, i.e., microbial population and color index. E-nose is therefore a suitable tool for monitoring
the storage of these products.
Discrimination of bacterial species is also of interest to the food industry although E-noses have not
been extensively investigated in this application. Rossi et al. [107] looked at the ability of the E-nose
Sensors 2010, 10 3903

to discriminate six sub-species of Staphylococcus and one of Micrococcus. These microbes are of
interest since they have been reported to be present in fermented sausages [108]. Factorial discriminant
analysis of the signals revealed that it was possible to classify 100% of bacterial species into their
respective groups. A cross-validation of the discriminant axes classified 90.5% of the bacterial strains
correctly.

3. Conclusions

Potential applications in odour assessment by electronic noses in the food area are numerous; they
have been used for quality control, monitoring process, aging, determination of geographical origin,
adulteration, contamination and spoilage. In most cases classification of samples was above 85%, but,
before these specific applications can become a reality, i.e., these laboratory-based assays are moved
into the industry, a number of challenges still need to be met; these are to properly assess various
characteristics of electronic nose performance, including drift, humidity influence, redundancy of
sensors, selectivity and signal to noise ratio. Although new sensor materials and designs, and
correction algorithms that can be applied for each sensor, are being reported, the major limitation of
currently available MOS sensors remains their independence and selectivity. Sensors with poor
selectivity affect adversely the discriminating power of the array. Additionally, with the technology
developed so far, it is unrealistic to envisage a universal electronic nose that is able to cope with every
odour type as specific data processing and, sometimes instrumentation, must be designed for each
application.

Acknowledgements

I would like to thank Stephen Trowell and Peter Watkins for their critical review of this paper and
specific comments which have improved the quality of this manuscript.

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