Trends in Analytical Chemistry 107 (2018) 142e150

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Trends in Analytical Chemistry

journal homepage: www.elsevier.com/locate/trac

Analytical systems and metrological traceability of measurement data

in food control assessment
Federica Bianchi, Marco Giannetto, Maria Careri*
Department of Chemistry, Life Science and Environmental Sustainability, University of Parma, Parco Area delle Scienze 17/A, I-43124, Parma, Italy

a r t i c l e i n f o a b s t r a c t

Article history: The article reviews food control systems in the framework of analytical quality assurance and metro-
Available online 7 August 2018 logical traceability of measurement data with focus on the analytical control of processes in the food
industry. Among approaches devised in response to emerging food safety and quality issues, as well as
Keywords: for food authenticity and traceability testing, those based on mass spectrometry are discussed as
Analytical testing powerful technologies for multiplex targeted and nontargeted screening methods. The article examines
Food control assessment
the role of spectral imaging techniques, isotope ratio mass spectrometry and biomolecular techniques for
Metrological traceability
assessing food authenticity, as well as the role of biosensors as high throughput screening strategies in
Quality control
Quality assurance
food control, underlying the power of chemometrics for analyzing data structures from multiple
analytical platforms. Quality control and quality assurance systems to guarantee robustness of analytical
processes and the role of metrological comparability as the prerequisite for reliability of measurement
results in food analysis are highlighted.
© 2018 Elsevier B.V. All rights reserved.

1. Introduction protocols. To assure the effectiveness of the control systems at

Effective food control systems are essential for implementation
of the legislation concerning public health and consumer protec-
tion taken into account the obligations of governments towards the
World Trade Organization. Food control measures are also critical in
developing countries to ensure safety and quality of food products
for international trade because of problems occurring along the
food chain.
As for the legal framework for food safety in the European
Union Member States, in 2000 the EU launched its White Paper on
Food Safety to create a transparent set of rules for appropriate food
and animal feed production and food safety control [1]. Originally
within the food safety legislative framework, the European Union
established a series of European Union Reference Laboratories
(EURLs) for food and feed. According to EC Regulation no. 882/
2004, EURLs have responsibilities to develop and validate test
methods, provide National Reference Laboratories (NRLs) with
details of analytical methods, including reference methods, and
support NRLs by organizing comparative testing combined with
adequate follow-up in accordance with internationally accepted
* Corresponding author. Fax: þ39 0521 905556.
E-mail address: careri@unipr.it (M. Careri).
national level, the Health and Food Audits and Analysis Direc-
torate of the Directorate-General for Health and Food Safety (DG
SANTE) has the task of carry out inspections in EU Member States
and in non-EU countries exporting to the EU to evaluate compli-
ance with EU standards. To coordinate food standards work on a
global level, the international food standards body (Codex Ali-
mentarius Commission) develops standards, guidelines and rec-
ommendations that serve as a reference for international food
trade to reduce food safety risks.
Food safety across the supply chain is also a high priority for
industry stakeholders, regulatory agencies and consumers. With
the emergence of food safety challenges and new health hazards
posed by contaminants, nanomaterials, biotoxins, hidden allergens
and residues in foods, food industry groups are establishing pro-
grams to identify and correct issues early in the production process
with the aim of reducing risk factors. In this context, advanced
analytical methods to address harmful substances are increasingly
becoming a centerpiece of food safety programs. Real-time process
monitoring with in-line and on-line analytical techniques (e.g. near
infrared spectroscopy, chemical sensors and biosensors) coupled to
multivariate data analysis allows the industry to continuously
measure core quality parameters in food manufacturing with the
final aim of producing safe high-quality products [2]. Further,
current development in the miniaturized instruments and wireless

https://doi.org/10.1016/j.trac.2018.07.024
0165-9936/© 2018 Elsevier B.V. All rights reserved.
 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150
communication allows instruments to be placed directly on in-
dustrial moving process equipment [3].
Food processors in enabling countries also have to withstand
problems with delivery of raw material on a timely basis, as well as
variations in overall quality due to a lack of infrastructure in the
producing areas. This calls for greater vigilance by the food pro-
cessing units and for food control activity to be implemented at any
stage of a long food supply chain. With the international trade, the
food supply chain has become more and more complex and food
safety risk management poses enormous challenges to the food
industry, since it has to consider all relevant aspects, including so-
ciological and cultural issues: poor food safety knowledge, particu-
larly in new migrant urban populations, and poor regulatory
infrastructures are limiting factors in setting emerging food safety
requirements. In this regard, the influence of multiple drivers on food
safety, from raw material to final consumption, including the hy-
gienic conditions of the production environment, has to be consid-
ered, the primary cause of food-borne illness coming from bacterial
contamination rather than from chemicals. High use of agricultural
inputs such as antibiotics, pesticides and chemical fertilizers, lack of
traceability and cross-contamination are also important challenges
facing developing countries in assuring safe food.
In this context, analytical systems aimed at food quality control
are vital for regulatory compliance and to ensure the quality, safety
and authenticity of food products. In particular, analytical testing of
food products can be performed to detect or confirm chemical and
microbial contamination, allergens, and to assess food traceability
and authenticity to identify and reduce economic fraud with the
ultimate goal of improving quality of food. In recent years, through
research, industry has improved a number of analytical methods
for guaranteeing food quality and safety with the further goal of the
detection of adulteration, being objective quality evaluation and
adulterant control in food products a key requisite for maintaining
the health of consumer. In this respect, it should be noted that a safe
quality product should be the result of adequate control at all stages
of the food chain rather than corrective action taken late in the
process. Therefore, preliminary analyses carried out by using rapid
screening methods could provide information about potential
contamination, thus reducing the number of samples submitted to
regulatory testing.
This review article presents latest techniques used for testing
food safety, quality and authentication with the emphasis on recent
analytical breakthroughs in this area. The significance of food
control measures to the success of the global food trading system
and the development of effective food control systems is also
highlighted. Attention is drawn to quality control and quality
assurance systems to guarantee the robustness of analytical pro-
cesses and the role of metrological comparability as the prerequi-
site for reliability of measurement results.
2. Analytical systems for food control assessment
2.1. Food safety and quality testing
As for the intentional or accidental contamination of food
products by undesiderable or undeclared ingredients, the devel-
opment and application of new analytical tools represents a great
potential for quality assessment, assurance, control and safety of
foods. Depending on the purpose of assay, screening and confir-
matory methods represent the most important approaches of
testing classification. As stated by Mun ~ oz-Olivas [4], “a screening
method is a process that extracts, isolates and identifies a com-
pound or group of components in a sample with the minimum
number of steps and the least manipulation of the sample”, thus
being very attractive for its cost-effectiveness and high-throughput
143
purposes in order to discriminate samples which contain no ana-
lytes above a threshold value (“negatives”) from those which may
contain residues above a specific value (“positives”). By contrast to
screening approaches, confirmatory methods are demanded to
provide full or complementary information enabling the analytes to
be unequivocally identified and quantified at the level of interest.
For large scale testing, different methods based on the use of bio-
sensors, microfluidic devices and imaging testing have been pro-
posed with the final aim of achieving quick responses by
performing on-site and/or on-line evaluations. To improve the
quality of surveillance, a host of multiresidue methods have been
also developed in order to analyze multiple substances simulta-
neously [5,6]. However, there are drawbacks in that some residues
and metabolites may not be included in the screening tests: several
pesticides such as highly polar pesticides and legally relevant
metabolites are not amenable to multiresidue procedures
commonly used by official control laboratories [7].
In the context of screening purposes, current improvements in
the field of biosensor technology for food quality and safety
assessment enabled the development of reliable, robust and se-
lective devices with high performance also in terms of sensitivity
and stability. In addition, last generation biosensors allow to carry
out time- and cost-effective multitarget screening assays in very
short times [8], playing a key role also in assessing food safety as
foodborne pathogen screening techniques [9]. In this regard, recent
advances in novel optical and electrochemical biosensors, nano-
and micro-scaled sensors and newly devised devices based on
novel bio-recognition elements such as aptasensors for detection of
salmonella pathogen in food have been very recently discussed in a
review article [10]. Among the novel approaches that allowed to
dramatically improve the performance and the applications of
biosensors for food quality and safety assessment, a fundamental
role is played by the use of nanostructured biocomposite materials
as sensing elements in biosensor technology (Fig. 1) [9,11]. In fact,
nanomaterials combine the enhancement of electrochemical and
optical signals with their high biocompatibility, so representing
exceptional electrode substrates for the efficient immobilization of
highly specific bioreceptors [12]. Microfluidic “lab-on-a-chip”
platforms have also emerged as promising tools for accurate and
high-throughput detection of mycotoxins and foodborne patho-
gens in foods, making portable and real-time biosensing of chem-
ical and biological hazards possible [10,13,14].
Over the last two decades, imaging techniques have been
established as analytical platforms for rapid, non-invasive and
non-destructive evaluation and inspection for food quality and
safety [15]. These techniques often require little or no sample
preparation, thus being particularly appealing for high-throughput
industrial applications. In particular, hyperspectral imaging tech-
niques, which combine capabilities of conventional imaging and
spectroscopy techniques allowing to obtain both spatial and
spectral information from the products, have resulted in many
successful applications in the food industry [16]. Among hyper-
spectral imaging techniques, terahertz (THz) spectroscopic imag-
ing has been recently proposed as innovative, non-destructive tool
to assess both the safety and quality of agri-food products [17]. The
highest performance of this technique for identifying low-density
foreign bodies embedded in foodstuffs if compared with X-ray
imaging, the reduced presence of scattering phenomena in com-
parison to conventional optical and near infrared (NIR) methods
and the use of a safer approach for both targets and operators if
compared to X-ray radiation are some of the main features of the
proposed technique.
When positive results from screening testing are achieved, the
use of confirmatory methods is needed in order to obtain the
univocal identification of unknown. In this context, techniques such
144 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150

Fig. 1. Examples of nanomaterial-based electrochemical biosensors for food safety. a) Procedure for fabrication of an immunosensor for ultrasensitive detection of aflatoxin B1 with
an enhanced electrochemical performance based on graphene/conducting polymer/gold nanoparticles/ionic liquid composite film on modified gold electrode with electrodepo-
sition [11]. b) Schematic performance of the electrochemical detection of target DNA based on CdSNPs-labeled oligonucleotides DNA probes for detection of pathogenic bacteria in
fresh beef [9].

as liquid chromatography-tandem mass spectrometry (LC-MS/MS)
and gas chromatography-MS/MS (GC-MS/MS) using tandem
quadrupole (QqQ) MS proved the most effective for the identifi-
cation of unknown compounds with the capacity to detect
chemical contaminants at very low concentrations, improving
confidence in the food supply [18]. In this regard, it has to be
considered that mass spectrometry is often called upon to address
legal and regulatory concerns for checking compliance with
maximum residue levels (MRL) in the case of determination of
contaminants and pesticide and veterinary drug residues [17].
Analytical strategies based on modern high-resolution (HR)MS
with time-of-flight (TOF) instruments are also effective both for
structure elucidation of unknowns and identity confirmation
of suspect substances, and for quantitative determination with
sensitivity approaching those for QqQ instruments in the field
of residue analysis [19]. In general, it is expected that the use of
benchtop instrumentation, integrating sample treatment and
analytical measurement, will favor the use of MS techniques for
routine analysis in food safety control [20,21].
Being capable of satisfying the requirements of high-throughput
purposes, recently, ambient MS has been proposed as valuable tool
for the analysis of different food matrices in their native ambient
with minimal or no sample treatment. Some of the most important
applications rely on the use of direct analysis in real time (DART)-
MS [22] (Fig. 2) and desorption electrospray ionization (DESI)-MS
[21,23]. In this regard, it has also to be noticed the increasing use of
HRMS to achieve the required sensitivity and selectivity, being able
to both discriminate among different target analytes and perform
retrospective evaluations on nontarget compounds [24]. However,
despite the widespread use of ambient MS techniques for qualita-
tive food safety and quality control, some drawbacks related to the
low performance in terms of repeatability/reproducibility are still
present, thus requiring the use of internal standards for quantita-
tion purposes. Finally, the problems related to the achievement
of very low detection limits can be overcome by using proper
sample treatment procedures before MS analysis, as demonstrated
in a recent study dealing with the development of molecularly
imprinted membranes for the direct electrospray ionization of
some pesticides in milk samples [25].
The rapid evolution in the analytical tools used to assess both
risks and potential benefits within the food chain has led also to the
development of non-targeted and broad scale approaches based on
omic techniques. In this context, proteomics and metabolomics
have significantly contributed to investigate the main aspects
of food quality and safety [26,27]. The application of omics
approaches in “Foodomics” has given rise to extraordinary oppor-
tunities in food research integrating molecular biology, food tech-
nology and sample preparation strategies together with advanced
analytical technologies (mainly omics tools) under a strong bio-
informatic environment (Fig. 3). The advances in HRMS have
allowed to achieve noticeable improvements in terms of sensitivity,
resolving power, robustness, tandem MS capabilities, thus being
very attractive for the scientific community. However, the omics
approaches suffer from important drawbacks, since most of them
are time-consuming, require trained operators, highly sophisti-
cated software for data processing and expensive instrumentation.
 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150 145

Fig. 2. Food quality and safety assurance in food supply chain with DART-MS and other ambient ionization (AI)-MS schemes [22].

By contrast, methods developed for food safety and quality testing
at industrial level need to be non-destructive, simple, suitable for
on-line and real-time applications.
Finally, special attention has to be given to the statistical methods
used for experimental data analysis. Conventional methods for food
quality and safety assessment based on chemical or microbiological
analysis followed by traditional univariate statistics such as ANOVA
are considered insufficient for some purposes. Being able to extract
valuable information from complex dataset, multivariate chemo-
metric methods play a crucial role in the comprehension of impor-
tant aspects dealing with food quality and safety problems [2,28],
enabling spectral data processing to extract the valuable information
related to the physical, chemical, and structural properties of sam-
ples when applied in spectral data studies [17]. A broad range of
chemometric tools including data reduction tools, regression tech-
niques and classification methods can be applied to obtain both
qualitative and quantitative information, being Principal Component
Analysis, Partial Least Square, Support Vector Machines some of the
most commonly used algorithms [29,30].
With the aim of achieving more reliable results, data fusion
methodologies, i.e. the combination of data from complementary
techniques, have been also proposed to enhance classification of
food and beverages and the prediction of their properties [31].
Taking into account the increasing availability of non-destructive
techniques, it can be supposed that the use of data fusion ap-
proaches will increase in the next future, thus allowing a better
prediction ability associated to the reduction of the uncertainty of
single results.

Fig. 3. Metabolomics workflow [26].

146 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150
2.2. Food authenticity testing
Food authenticity testing is an important component in many
quality and safety programs, the ability to trace and authenticate a
food product being of major concern to the food industry. Access
to analytical tools is therefore essential to verify food integrity,
requiring continuous development in the identification of molec-
ular markers, data acquisition and modeling. Targeted analytical
approaches are useful when the chemical compound is known and
specifically screened. Conversely, improvements in analytical
instrumentation and data analysis software allowed the develop-
ment of nontargeted testing methods aimed to create a “finger-
print” of an ingredient or food product for assessment of possible
adulteration and contamination [32,33].
During the past two decades, omics technologies with bio-
analytical platforms have been demonstrated as a powerful
analytical tool not only for food quality and safety assessment
[26,27], but also for the detection of food authenticity and integrity:
genomics, proteomics, metabolomics and lipidomics are the
molecular-based technologies which have the potential for allow-
ing a significant reduction of food fraud (Table 1) [34].
Among omics technologies, measurement issues associated
with molecular and mass spectrometry analysis of food matrices for
detection of food fraud were recently investigated, with a timely
reassessment of their quantitative potential [35]. In this regard, a
proteomic approach via multiple reaction monitoring mass spec-
trometry has been successfully proposed to devise a multiplex
targeted method for the rapid detection and relative quantitation of
the adulteration of meat with that of an undeclared species, the
approach being based on the use of corresponding proteins from
the different species under investigation and selected peptide
markers for species detection [36].
Other proteomic and metabolomic studies have been proposed
as effective tools to trace food adulteration [26,37]. In this context,
HRMS is often required to obtain reliable data for the subsequent
steps based on chemometric evaluation (multivariate data analysis)
and marker identification. Obviously, both the availability of bio-
informatic tools and data preparation with model generation/vali-
dation are crucial for successful results in which a multivariate
model has to be proposed for real applications [38,39].
In order to achieve the development of high-throughput ap-
proaches suitable to detect biomarkers for ensuring the authenti-
cation of food and to screen a great number of samples with
minimal sample treatment, ambient MS-based methods have also
been applied, being DART, DESI, easy ambient sonic-spray ioniza-
tion (EASI) some of the most used ion sources [40]. All these
ambient MS techniques rapidly generate a plethora of finger-
printing data to be submitted to a specific chemometric treatment
for food authentication requiring no sample preparation and min-
imal sampling time. In addition, being these techniques adaptable
Table 1
A brief definition and description of the omics technologies used for the detection of food authenticity and integrity [34].
Omics approaches Description
Genomics The study and assessment of variability and function of DNA
sequences
Proteomics The study of structure, function and abundance of different proteins
and peptides (or complexes), post-translational modifications
(PTM) in a system
Metabolomics The comprehensive and systematic study of low molecular weight
compounds (metabolites) involved in metabolism in a system
Lipidomics The study of pathways and networks of different lipid species in a
system
to miniaturization [41], in the near future it is possible to foresee an
increase in their use also for on-site real-time analysis.
Besides to MS-based methods coupled with multivariate data
analysis, other technologies have also been shown to identify
potentially adulterated materials. Isotope ratio mass spectrometry
(IR-MS) has proved to have great potential for assessing the
authenticity of food of animal origin, being capable of determining
geographical origin, animal diet and the technological process.
Technological progress has led to an increased use of hyphenated
techniques for measuring isotope ratios using IR-MS combined to
GC or to elemental analysis to improve the determination of the
origin of a variety of food products [42]. On the other hand, it
should be pointed out that the main drawback of the application of
IR-MS technique is the need of databases for each food commodity,
which are expensive to create and to maintain in terms of both time
and financial costs.
Other analytical methods used for species identification and
authenticity of foods rely on protein and DNA analysis [43]. Among
DNA-based procedures, methods based on the highly specific
amplification of one or more DNA fragments by means of poly-
merase chain reaction (PCR) have been proposed as useful means
for identifying species of origin in foods, as well as undeclared
allergenic ingredients and genetically modified organisms (GMO),
presenting a high potential due to their high specificity and sensi-
tivity. As the principal drawbacks of PCR-based methods are as-
cribable to the long times and high costs involved in the analytical
process, among novel DNA-detection technologies, electrochemical
or optical genosensors are becoming more and more a valid alter-
native to other screening assays for rapid and efficient screening
tests aimed to detect and quantify DNA sequences ascribable to
GMOs or to specific cultivars in food traceability and authenticity
testing [44]. The high impact of sensing devices for food authen-
tication is undoubtedly related to the recent advances in the inte-
gration of compact and portable sensors with smartphones, leading
to the development of “hand-held” screening tools characterized by
test rapidity, low cost, ease-of-operation and data management.
These devices combine high reliability of chemical sensors with
minimal equipment and user's involvement through mobile per-
sonal tools (e.g. smartphones and tablets) [45]. In the field of
smartphone-based food diagnostic technologies, the Internet of
Things (IoT) approach is indeed promising, as the research outputs
are quickly capitalized on new start-up companies.
Finally, electronic noses and tongues, frequently associated to
multivariate chemometric techniques for the deconvolution of
big-data inputs, are also extensively and effectively used for food
authenticity and adulteration assessment (Fig. 4) [46].
Chemical multisensor systems are one of the most promising
approaches for in-line process control aimed at direct, rapid, and
accurate determination of several target compounds, with minimal
or no sample preparation and reagent consumption. The innovative
Approaches and technologies
Whole-genome sequencing (WGS), Next generation sequencing
(NGS), Amplified fragment length polymorphism (AFLP), Single
nucleotide polymorphism (SNP), Simple sequence repeat (SSR)
Two-dimensional gel electrophoresis, MALDI-TOF-MS, LCeMS and
high-resolution tandem mass spectrometry
Metabolic fingerprinting (FT-IR and Raman spectroscopies),
Metabolic profiling (GC/LCeMS, NMR), Targeted metabolomics
analysis
Lipid profiling (GC/LCeMS, NMR), Shot-gun MS, Lipid fingerprinting
(MALDI-TOF-MS), Ultra-performance LCeMS (UPLCeMS)
 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150
Fig. 4. Schematic representation of (a) an electronic nose and (b) an electronic tongue [46].
approach combining the outputs of multiple artificial sensors,
called “sensor fusion” and already described for food quality
assessment [31], has been applied to a wide range of food and
beverages to improve authentication of food, enhancing signifi-
cantly the performance of the same instruments when used indi-
vidually [47].
3. Analytical quality assurance and metrological traceability
of data
In addition to developments in food science and technology, with
the liberalization of food trade and improvements in transport, new
legal requirements in mainly developed countries relating to trace-
ability have recently been implemented. Traceability throughout
food chain combined with traditional food safety programmes re-
quires the development of reliable analytical methods capable of
detecting harmful residues and contaminants, thus diminishing risk
and protecting the consumer. To this aim, analytical methods used
by enforcement laboratories for the implementation of legislation
must be subject to validation procedures. The prerequisite for reli-
ability of measurement results is also comparability on the basis of
known uncertainties which in turn are based on traceability to
recognized references [48].
Measurement uncertainty and traceability are essential for the
evaluation and comparison of quantitative test results. Regarding
food safety issues, particularly in the case of determination of
mycotoxins that are heterogeneously distributed, the underlying
problem is the large variability and uncertainty associated with
sampling and sample preparation procedures that may lead to
unrealistic results [48]. Sampling and subsampling procedures
should be designed according to the mycotoxin distribution.
Another important consideration in risk management is the
method used for mycotoxin detection. Although the uncertainty is
not as high as in the sampling, reliable analytical methods are
required to determine mycotoxin presence in foods.
As for food safety assessment of pesticide residues, as well as of
environmental and industrial contaminants showing chemical or
other similarity to pesticides, sampling and analysis of residues
play an important role in testing compliance with legal limits.
147
The uncertainty of the determination of pesticide residues in test
portions depends on the method used [49]; on the other hand,
because of their large variability in agricultural food products, un-
derestimation of sampling uncertainty may have severe conse-
quences in testing compliance of commodities with legal limits.
Concerning food authenticity testing, standardization and vali-
dation of robust analytical methods within EU to support integrity
of food chain are current challenges. As already discussed, methods
based on PCR or mass spectrometry for detecting the presence of
particular nucleic acid or peptide/protein sequences have been
shown to be specific and sensitive, but they are affected by a high
measurement uncertainty and scarce reliability when applied to
complex food matrices [35]; therefore, reduction of measurement
uncertainty in those procedures and of variability of DNA extrac-
tion/amplification is demanding and has become a goal for many
laboratories. In this regard, when validating quantitative PCR-based
and proteomic methods attention has to be paid on the various
factors that can impact on the measurement uncertainty of a result
associated with those approaches used in detection of food
fraud [35]. Also, when using IR-MS it is necessary to know the
measurement uncertainty to make meaningful origin assignments:
in this way the differences in elemental concentrations or isotope
ratios in products from different geographical origins can be
considered as statistically significant or not and the isotopic ratios
can be used as significant predictors in determination of the
geographical source of food commodities.
Traceability is an important part of the quality assurance applied
in a laboratory. To ensure international metrological comparability
and traceability of results to international reference standards,
mutual recognition of analytical measurement results is required.
The Comite  International des Poids et Mesures Mutual Recognition
Arrangement (CIPM MRA) is the framework through which Na-
tional Metrology Institutes demonstrate the international equiva-
lence of their measurement standards leading to the internationally
recognized Calibration and Measurement Capabilities (CMCs) of the
participating Institutes. Approved CMCs and supporting technical
data are publicly available from the CIPM MRA database (http://
www.bipm.org/en/cipm-mra/), which has become an essential
reference for the accredited laboratory community amongst others.
148 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150
In order to establish an international arrangement between mem-
ber accreditation bodies, the International Laboratory Accreditation
Cooperation (ILAC) MRA promotes acceptance of results providing
significant technical support to the calibration, testing, and in-
spection results of the conformity assessment bodies that are sig-
natories to the ILAC MRA. By removing the need for additional
calibration and testing, technical barriers to trade are reduced. In
this way the ILAC MRA promotes international trade and the free-
trade goal of “accredited once, accepted everywhere” can be real-
ized. Under ILAC MRA the Member States shall ensure the quality of
the results of the analysis of samples taken pursuant to Directive 96/
23/EC, by monitoring tests and/or calibration results according to
the International Standard ISO/IEC 17025:2005, which is designed
for the accreditation of Testing and Calibration Laboratories. As for
food control, Authorities may only designate laboratories that
operate and are accredited in accordance with the European stan-
dard EN ISO/IEC 17025.
In the context of laboratory accreditation, the importance of
validated methods as well as of internal and external quality con-
trol is well recognized. As already discussed, the establishment of
EURLs and NRLs should contribute to a high quality and uniformity
of analytical results. This goal can be achieved by the application of
validated analytical methods, ensuring that reference materials are
available, and the organization of comparative testing. Great effort
has also been made to set up harmonization documents for method
validation and quality criteria for the identification and confirma-
tion of residues and contaminants by MS-based methods particu-
larly for food safety purposes (Fig. 5) [50,51]. To obtain reliable
analytical data an effective measurement assurance requires also
that the equipment must be used properly and personnel should be
both qualified and competent to undertake the task.
EU Member States are responsible for enforcement of the EU
agri-food chain rules including EU legislation on official controls
(Regulation No. 882/2004). The official control should be performed
using appropriate techniques including routine surveillance checks
Fig. 5. Demonstrating fitness for purpose of qualitative methods. Underlined items
could benefit from further clarification or additional resources in the mass spec-
trometry community [51].
and more intensive controls such as inspections, audits, sampling
and sample testing. Sampling and analysis methods used in official
controls shall comply with relevant Community rules or with
internationally recognized protocols in the absence of such rules or
with other methods fit for the intended purpose in the absence of
internationally recognized protocols. In this context, laboratories
shall comply with the provisions of Article 12 of Regulation No
882/2004 and shall be able to demonstrate that they use internal
quality control procedures. Quality control procedures should also
include participation in external Proficiency Testing (PT) Schemes
which comply with the International Harmonized Protocol for the
PT of Analytical Laboratories developed under the auspices of IUPAC/
ISO/AOAC. The role of the EU is to assure that the control systems at
national level are effective. This is the task of DG SANTE.
Quality control and quality assurance systems are established to
guarantee the robustness of analytical processes. Such systems
make use of criteria related to minimum sampling variability,
representative sampling, recovery rates, minimum number of ‘sus-
pected false negatives and positives’, linearity of the calibration
curve, within- and between-laboratory repeatability and repro-
ducibility of results, etc. Representative sampling is of primary
importance. If samples are improperly collected and mishandled or
are not representative of the sampled lot, the laboratory results will
be meaningless. To ensure that the final laboratory results are cor-
rect, the quality assurance program incorporates those planned and
systematic laboratory activities that guarantee the accuracy and
defensibility of testing results. Besides to the development of
harmonized systems of measurement, the high degree of consis-
tency in experimental data required for the implementation of
European Directive on food control can be achieved by the appro-
priate use of reference materials (RMs) and certified reference ma-
terials (CRMs). CRMs are key tools for achieving traceability of the
measurement results, proving accuracy of methods and demon-
strating proficiency of laboratories. CRMs also provide an important
milestone in the development of robust analytical processes, which
are composed of screening and confirmatory procedures. They are a
cost-attractive tool for validation and quality control of test kits and
sensors. The International Organization of Legal Metrology sets out
guidelines with a view to facilitating a wider use of CRMs for legal
metrological control also in the field of food safety. The availability
of CRMs is still quite limited and does not fulfill the demands of the
laboratories. Therefore, it is essential to encourage worldwide the
production of new CRMs and the accreditation of reference material
producers. Quality control procedures should also include partici-
pation in external Proficiency Testing Schemes, which ensure that
technical competence is also maintained in the accredited labora-
tory. The role of the EU is to assure that the control systems at na-
tional level are effective thanks also to high-performance reference
laboratories and to assess compliance with EU standards in the food
safety and quality sector within the EU and in third countries in
relation to their exports to the EU, thus ensuring a high level of
protection of human health regarding the food industry.
4. Conclusions and future trends
Analytical techniques and analytical systems made important
contributions to the food industry, with new tools for investigation
and analysis for food safety and quality control. There are also many
emerging techniques available that can provide traceability infor-
mation useful for food authentication purposes. Especially when
used in combination with the aid of chemometrics, that are crucial
to analyze the vast amount of data generated by modern analytical
platforms, these techniques can provide extremely powerful tools.
In the last decades there has been a rapid growth in the use of
frontline technologies such as ambient mass spectrometry for
 F. Bianchi et al. / Trends in Analytical Chemistry 107 (2018) 142e150
detection of food adulteration if compared to conventional tech-
niques commonly used to trace food fraud and investigate food
safety. In this regard, developments in miniaturized mass spec-
trometers have demonstrated their potential also in determining
food adulteration. In general, miniaturization of analytical systems
will remain under development including newly emerging tech-
nologies able to offer platforms with great automation and multi-
plexing capabilities. These multiplexed analytical techniques are
expected to provide control agencies and food industries with new
possibilities for improved, more efficient monitoring of food and
environmental contaminants. The application of novel sensors as
well as of chemical multisensor systems to food control is also
expected to play a key role in future because of the high sensitivity,
portability and real-time analysis offered by lab-on-a-chip plat-
forms affording to monitor early spread of chemical and biological
hazards in food products before the outbreaks can occur.
The globalization of food trade and national as well as interna-
tional food safety regulations has produced an enormous demand
for comparability of analytical results independent of temporal or
spatial borders. In this context, the objectives of ensuring an
adequate level of food quality and safety can be pursued by
implementing quality assurance measures along the entire food
chain, but also to devise fast on-line monitoring methods or at-line
analytical techniques in response to a food safety emergency as
constituting a serious foodborne risk to public health that requires
urgent action. In such instances, reliable data derived from vali-
dated analytical methods are required to enable industry stake-
holders and regulators to make sound scientific decisions.
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