Quality Control and Food Safety

Innovative Analytical Methodologies Control
of Quality and Food Safety

Partners

 

Consortium as a whole

 

Technical and scientific expertise.The development and application of analytical methods for food analysis is a research line common for all the participant groups. But under this line, the different groups and researchers of each group possess different knowledge, analytical techniques and available equipments, and also they carry out their research on different applications.

A multidisciplinary focus is especially necessary in food analysis. Safety and quality represent different concepts and aims in this program. But both knowledge and resources of all participants detailed below will be useful in order to achieve the proposed aims.

 

Potential for future partnership

In general, collaboration among groups will be focussed on the exchange of knowledge and resources listed in the previous section.

·     Knowledge about methods: The development of a method is a detailed work which requires scientific rigor. The collaboration among groups will make it easier.

·     Knowledge about foods: A safety or a quality problem can appear in a food in which the responsible group does not possess previous experience. The support from experienced groups in this matrix will be crucial to obtain good results.

·     Knowledge about optimization and validation:The experience of some groups in statistical models will be useful for the selection of the appropriate technique to be used and to interpret the obtained results.

·     Techniques and equipments: In this section, not only the sharing of equipments among groups but also to provide and to receive an specific formation at high level about food analysis will be of the utmost importance in the Program. The accumulated experience of all the groups in the study and the solution of problems of Food Technology should be considered as an added value. All the existing infrastructures, human resources and real synergisms can be understood as an opportunity to solve complex aims difficult or highly expensive to achieve by other methods.

 

Research groups

-      Dpto. Análisis Instrumental y Química Ambiental. IQOG. CSIC

-     Grupo de Calidad, Seguridad y Bioactividad de Alimentos procesados térmicamente, OXILIPID y BIOCELL.  ICTAN. CSIC

-      Dpto. de Química Analítica. Facultad de Químicas. UAH

-      Dpto. de Química Analítica. Facultad de Ciencias Químicas. UCM

-      Grupo de Técnicas y Métodos de Análisis Químico. Facultad de Ciencias. UNED

 

Group CSIC-AI: Instituto de Química Orgánica General - AIQA

 

The investigation of this group is based on the innovation and development of instrumental analytical techniques, mainly of separation (gas and liquid high-resolution chromatography) coupling to mass spectrometry and on the application of these techniques to the study of samples of interest from environmental, food and health areas. The overall objective of our research is to develop new techniques and analytical methods of separation that provide high sensitivity, selectivity, speed, reliability and low cost in order to apply them to solve problems related with the environment, with the safety and quality of food and with health issues.

At present, we are working on several topics related to program I+D we are appliyng. On the one hand we are working on modelling studies of the chromatographic behavior and in the development of methods based on GC and GC-MS for the study of organic compounds (volatiles,, carbohydrates and other molecules) in food, plants and soils.

In addition, the group has extensive experience in the study of food components using different techniques such as supercritical fluids, SPME and SDE systems for extraction analysis and multidimensional chromatographic (RPLC x GC) technique for final determination. In addition, the group has collaborated in the development of a patent for the interface TOTAD which is marketed by the Konik company.

 

By other hand, we are working on the development and validation of analytical methodologies for the determination of organic compounds at trace levels in food samples. Such investigations were started in the early 70’s for the analysis of apolar toxic contaminants such as PCBs and organochlorine pesticides in biotic samples and food.

In the late of the 80’s studies concerning to the determination of PCDD / Fs in these complex matrices were begun, since that analysis is carried out continuously in our laboratory. More recently, the research field has been expanded to include other persistent organic contaminants such as PAHs, flame retardants (PBDEs, HCDD), enantiomers of chiral PCBs and toxaphene and pesticides, always in environmental and food matrices of high complexity.

As can be seen in the CV of the applicants investigators, some of these investigations have been addressed toward the miniaturization of some of these analytical methodologies as well as research on new techniques for sample preparation. All of them with the aim of developing new analytical procedures, prior to the development of analytical instrumentation that allows the quantitative analysis and fast screening of Persistent Organic Compounds from different foodstuffs, a field in which our group has been a pioneer both nationally and internationally.

 

Group CSIC-AA: CSIC - Instituto de Ciencia y Tecnología de los Alimentos y Nutrición

 

CSIC-AA group is formed by researchers specialised in food chemistry, processing and human nutrition. Members of the groups are a national reference in the evaluation of new food-derived toxicants which are induced after thermal processing, as acrylamide. The research group has developed a validated methodology for analysis of acrylamide in different food matrices by lc-ms, but also, an approximation of risk assessment for the estimation of dietary intake of acrylamide to Spanish population. Hereby researchers in CSIC-AA are members of different panels of risk evaluation to exposure of acrylamide from diet at the European Food Safety Agency (EFSA). Another example of the relevance of the investigation developed is the invitation to take place in the new group (CEN/TC 275/WG13) supported by CEN (European Committee of Normalisation) with the ain to develop official procedures for analysis of process formed contaminants. In addition, the linkage to the productive sector is highlighted in the development of the European project ICARE (Impeding the formation of neoformed contaminants in processed foods 2006-2009), as well as the participation in the just concluded COST927 action (Health implications of thermally processed foods) (http://www.if.csic.es/proyectos/cost927/index.htm).

 

Research group has been focused in the evaluation of quality and safety of processed foods. One of the most important reactions which take place during thermal processing of foods is the so-called Maillard reaction. In the former 5 years, several methodologies which are rapid, robust and sensitive have been developed for the evaluation of new substances with implications in the biological and nutritional quality of foods (see cv2009_Morales_Navas_Francisco). Briefly, liquid chromatography and capillary electrophoresis has been used as coupled to ms and DAD detection.

In addition, CSIC-AA covers other key chemical reaction in food such as the lipid oxidation (chemical and analytical aspects), and particularly during the deep-fat frying. It is noteworthy to highlight the contribution of the analytical evaluation of frying oils in collaboration with professor Dobarganes (CSIC). Study of the kinetic of formation of compounds of lipid oxidation and the development of new analytical strategies are also considered.

On the other hand, CSIC-AA has also a wide experience in studying bioavailability, metabolism and biological effects of diverse food components in vivo (polyphenols), and in cell cultures (polyphenols, Maillard reaction products, organic and inorganic selenium species, etc). Moreover, CSIC-AA posses the necessary experience and know-how to deal with toxicity studies in animal models and in different cell lines.

Recently, Instituto del Frio got the ISO9001 (ER-0366-/20080, AENOR) certification with the scope “Management and development of research projects and contracts in the area of Food Science and Technology and Nutrition”. In parallel, the labs in CSIC-AA have already started the way to the accreditation in various analyses, for example acrylamide in cereals and derivatives.

 

 

Group UAH-QA: Universidad de Alcalá de Henares - Química Analítica

 

The research group of Analytical Chemistry of the University of Alcalá (UAH-QA) headed by Prof. Dr. Marina has developed in last years an intense research activity of national and international relevance in the fields of chiral analysis and control of the quality and safety of foods. These works have been focused mainly on the development of rapid and sensitive analytical methodologies with low economical and environmental costs with special emphasis on the improvement of the automation, miniaturization and hybridization of analytical systems, several of the most current tendencies in the field of analytical chemistry. The developed methodologies were based on the study of the protein and peptide fraction, and on the enantiomeric determination of amino acids in foods in order to establish the real compositioin of foods and to propose new markers enabling the control of the quality and safety of foods as well as the accomplishment of legal regulations. The UAH-QA group is an expert in the use of chromatographic and electrophoretic separation techniques, especially, High-Performance Liquid Chromatography (HPLC) and Capillary Electrophoresis (CE) with optical as well as mass spectrometry detection. The results obtained have conferred this group an international prestige in this field as shown by the high number of invitations received to participate in international and prestigious books and special issues of the most important journals in the field of analytical chemistry and food analysis.

 

Most relevant results obtained in the last 5 years in relation with the programme.

 

·  Innovative and rapid analytical methodologies have been developed for the separation and determination of vegetable proteins in foods by HPLC as well as micro/nano-HPLC and Capillary Electrophoresis with optical and mass spectrometry detection. With this aim, sample preparation has been considerable simplified and new generation (high-velocity) stationary phases have been employed in HPLC in order to drastically reduce analysis time in the analysis of high molecular mass proteins.

·   Vegetable proteins investigated included soybean, maize, rice, wheat, etc. and the developed analytical methodologies enabled the characterization of soybean and maize transgenic and non-transgenic cultivars, and their protein fractions as well as the determination of several of the vegetable proteins investigated in vegetable foods, meat and bakery products, dairy products, etc. A marker peak has been proposed for the detection of adulterations in meat products with soybean proteins and the marker proteins have been identified by a proteomic study by multidimensional chromatographic techniques coupled to mass spectrometry.

·  New strategies have been designed in order to improve the sensitivity in chiral Capillary Electrophoresis when using optical as well as mass spectrometry detection. The combination of sample preparation strategies, such as derivatization, with in-capillary sample preconcentration and enhancement of the detection in both cases, has enabled to obtain the lowest detection limits reported in chiral analysis by capillary electrophoresis. This has enabled for the first time to propose analytical methodologies for the unequivocal determination of enantimers of amino acids in foods with a complex matrix.

 

 

Group UCM-QA: Universidad Complutense de Madrid - Química Analítica

 

The group has a wide experience in the next research lines:

·   Analysis of trace elements in complex matrices, food and environmental samples, using atomic detection systems. Development of several analytical methods that provide important improvements both for the selectivity and detection limits.

·    Trace element speciation by coupling chromatographic techniques with high sensitive detectors. Our research group has pioneered the speciation of Se and Sb and has designed several instrumental coupling systems between techniques.

·  Phytorremediation: Evaluation of the ability of certain plants to concentrate toxic metals. Bioaccumulation and biotransformation of essential metals. Similar research has been developed on fish (specially in the case of Se).

·    Preparation of functional foods enriched with Se (yogurt, plants, fish). We are recently evaluating the bioaccumulation and biotransformation of selenium together with other elements of interest, their incorporation to proteins and the interaction between different elements, the antioxidant, antistress and anticarcinogenic activity of functional foods enriched with Se.

·     A parallel study is currently under development to evaluate the incorporation of Pt or W to proteins and its bioaccumulation after administration of anticancer and antidiabetic drugs, respectively. This evaluation is being done both in vivo and in vitro. Different nefroprotecting agents are being evaluated to prevent secondary effects of cisplatin treated patients.

·   Development of new methodologies for the evaluation of the enrichment of different emerging pollutants by zebrafish embryo, and the extrapolation of results to other living organisms. This research line involves the development of miniaturized sample treatment methodologies for the determination of organic pollutants, pharmaceutical products, drugs, metals and nanoparticles.

·     Coupling of laser ablation to ICP-MS for the determination of trace elements in biological samples

·     Development of new imprinted polymers as selective sorbents in solid phase extraction and selective stationary phases in HPLC or capillary electrochromatography for the determination of organotin compounds, pesticides and pharmaceutical products.

 

Group UNED-QA: Universidad Nacional de Educación a Distancia - Ciencias Analíticas

 

The research group has extensive experience in developing analytical methodologies for the determination of organic compounds (pollutants, drugs and various toxic) in environmental samples and foods. In the past decade research has focused on developing new methods of sample treatment (extraction, purification, preconcentration and clean-up) based on the selective use of natural molecular receptors (immunological receptors) or synthetic (MIPs) for the determination of different analytes.

In addition, the research team has proven experience in analytical techniques such as liquid and gas chromatography using different detection systems, being demonstrated by the supervision of four PhDs in this field and other research works (DEAs), a large number of articles published in international journals (Science Citation Index), as well as numerous contributions on national and international congresses. Staff who joined the group also has great experience in the field of luminescent host immunological techniques and chemometric methods, and has worked together since its formation on the same lines of research drawing on the experience separately.

In recent years, the research group has participated in several research projects funded by the MEC (CTQ2006-15027) and Comunidad Autónoma de Madrid (S-0505/AGR-0312), the latter being co-ordinated in which has collaborated with other groups of Spanish research, such as the group of Dr. D ª. José M ª González (CSIC), the group of Prof. Dr. Carmen Cámara (Universidad Complutense de Madrid, UCM) and the group of Prof. Dr. Ms M ª Luisa Marina (Universidad de Alcalá de Henares, UAH), among others. The main objective of these projects has been the development of analytical methodologies for the determination of contaminants in food samples and food quality assurance.

The projects funded in recent years have enabled the requesting group the development and validation of analytical methods using simple and selective sample treatments for the determination of macrolide antibiotic and estrogens in water samples and food as well as the possibility of a new line of investigation for the determination of other food toxics like some azo dyes. In addition, the research group has acquired a great experience working with other groups in coordinated projects, both in assessing the quality of food in the determination of these pollutants in low concentrations in complex matrices. As mentioned, the purpose of expanding the scope of the research work, the group has launched a new line of research that aims to establish a methodology for monitoring residues of azo dyes in food samples.

Our group, based on its experience in the methods of samples treatment, has provided various training courses in this area for teachers of High School of the Community of Madrid (Sampling and Processing of Samples, QUI02CM07, 30 hours, 3 credits, 2007), as well as training courses for researchers (New Methodologies for the Analysis of Xenobiotics in Food, 60 hours, 2007), organized by ANALISYC Programme.

The experience gained in these earlier studies makes the possibility to focus this project on safety and food quality control. Therefore, our main objective is to develop analytical methods for samples treatment, which allow a selective, sensitive and easy way to identify several contaminants (pharmaceuticals, estrogens and azo dyes), including some of them in the lists of emerging contaminants in food. The determination of these compounds will introduce in the laboratories of food quality a simple and efficient alternative to carry out routine analysis.

This research group has been recognized as Consolidated Research Group by the UNED (Group of Techniques and Methods of Chemical Analysis (GTyMAQ) Ref: G30E12). The scientific results of the research group have resulted in numerous publications (43), PhDs (9, five of them developing) and other research works as Diplomas of Advanced Studies (8) as part of the initial research of o doctoral thesis.

 

Laboratories

 

-     Unidad de Servicio de Técnicas Analíticas, Instrumentales y Microbiológicas, ICTAN. CSIC

-     Dpto. Química Inorgánica y Analítica. URJC

 

 

Laboratory 160: Unidad de Servicio de Técnicas Analíticas (USTA)

 

The Analytical Service Unit is composed of 5 areas of which the work within the programme will be performed in the area of Chromatography, Colorimetry and Spectrophotometry. The responsible of the area is a specialist on the corresponding analytical techniques (see CV) y coordinates activities such as analytical applications. Besides, the area counts with two assigned analysts. The continued qualification is one of the premises of the quality plan of the Unit and, thus, the staff members assist regularly at courses on the mentioned techniques.

The area counts with the following equipment of relevance for the programme: HPLC-MS (1), HPLC-DAD (1), GC-MS (2), RMN, FT-NIR.

The Unit has carried out analytical support for numerous users, thus contributing results to many research projects y contracts with industry. Regarding the programme, the analytical support by LC-MS and training of members of the CSIC-AA staff within the European project ICARE should be emphasized. Technically it is relevant to emphasize the participation in several proficiency tests organized by the IRMM (Institute of Reference Materials and Measurements) on the determination of acrylamide in potato crisp samples obtaining very satisfactory results with the LC-MS of the Unit (z-score -0.5). All activities of the Unit are integrated in a quality system, partly the management system of the Instituto del Frío itself (ER-0366/2008) according to the Standard ISO 9001, partly another system based on the Standard ISO 17025 aiming of guaranteeing the technical competence of the Unit in the performance of some of the analysis.

The Service Unit offers a catalogue with a large number of services on food analysis. Of the offered services the most important are: Gas chromatography-mass spectrometry (GC-MS), Gas chromatography (GC-FID), Liquid chromatography-mass spectrometry (LC-MS), Ion chromatography, Analysis of nitrogen/protein, Analysis of elements by atomic absorption spectrometry, Basic analysis (ash, dry extract etc.), Microbiological analysis and identification of microorganism, Supply of strains of microorganisms, Thermal analysis, Verification and calibration service (mass, temperature, absorbance, wavelength) according to verification and calibration plans, Maintenance of common equipment according to maintenance plans, Courses and training and User attention (technical advice).

The service vocation of the Unit facilitates the interaction with research groups, not only of the institute itself and the CSIC but also University laboratories, other public research institutions, private laboratories and companies that belong to the agro alimentary sector that have firmed research agreements and/or contracts with certain working groups. On the other hand the Unit collaborates with the company Agilent Technologies which makes demonstrations for new clients on the LC-MS in return for an advantageous maintenance contract for the laboratory.

 

Laboratory URO520: Electroquímica y Técnicas de Separación URJC - Departamento de Química Inorgánica y Analítica

 

The Electrochemical and Separation Techniques laboratory (LETS) is a new associated laboratory of applied investigation. The research group has 13 members of Analytical and Inorganic Chemistry Areas in the ESCET. The investigation of this laboratory is based on: Development of new hybrid mesoporous silica applications for the SPE, HPLC, CE and electro analytical applications. Development and validation of analytical methods for the separation of quiral compounds by HPLC-DAD, HPLC-MS y CE. Development and validation of analytical methods for the separation of emerging toxics in waters and foods by HPLC-DAD, HPLC-MS y CE. Development of new hybrid mesoporous silica applications for preparation of carbon paste modified electrodes for heavy metals analysis in waters by AdSV.

At present the LETS is collaborating with several investigations groups, not only belonging to the URJC but also with other Universities. It is important to mention the close collaboration with Professor Maria Luisa Marina from the UAH, with the Profesor Antonio Otero from the UCLM and with Professor Pilar Gomez-Sal from the UAH.

It is important to highlight the collaboration that the LETS has in place with the private company Beckman Coulter, consisting in CE equipment demonstrations for new customers and also supporting a scholarship in a joint research work about the development and validation of analytical methods for estrogens determination in water and food.

The requested equipment in this program as well as the existing ones at the LETS will be available for all the research groups participating in it or not and to private companies according to the technical services. In relation with the program objectives, the mission of the laboratory will be to offer scientific and technical support mainly to UAH-QA group in Objectives 1 and 5. In relation with the development of new analytical methodologies for the detection of emerging toxics in food (Objective 1), the LETS will be offer support in the preparation and characterization of mesoporous silicas as SPE sorbents and HPLC and CE stationary phases. In relation with the Objective 5, related with development and optimization of sample preparation methodologies, the LETS will be support in the preparation, characterization and evaluation of hybrid materials as heavy metals adsorbents.

On the other hand, it is necessary to adapt methodologies to good laboratory practice criteria and their possible implantation in a quality system. In this point the LETS has the objective of the implantation of this quality system in collaboration with the CAT and 160 laboratory.

 

 

Associated groups

 

Associated Research Groups

 

AR-GAMA, del Gobierno de Aragón, centra su investigación en la propagación y cultivo de plantas. Posibilidad y evaluación de la obtención a gran escala.

UCLM-OENNAT, Univ. Castilla- La Mancha. Su investigación en el campo de los alimentos, sobre todo en aspectos analíticos aplicados a vinos y productos naturales.

CSIC-IQAB, del IDAEA, CSIC, con sede en Barcelona, centra su investigación en el estudio del comportamiento y detección de contaminantes tóxicos persistentes en alimentos

 

Offical organisms

AESAN, Agencia Española de Seguridad Alimentaria y Nutrición

Consejería de Sanidad de la Comunidad de Madrid

CERSYRA, Centro Regional de Selección y Reproducción Animal, Valdepeñas (Ciudad Real)

FIAB, Federación Española de Industrias de la Alimentación y Bebidas

 

Companies

 

Food companies 

Bioserch, S.A.

Grupo leche Pascual

Campofrío alimentación S.A.

Ganadería Priegola S.A.

Grupo Mahou-San Miguel, S.A.

FUNDISA, Fundación Ibérica para la Seguridad Alimentaria

Fundación LEIA, Centro de desarrollo Tecnológico

Plataforma Tecnológica Española de los Alimentos Food for Life Spain

Kemira OYJ

 
 

Analytical Instrumental companies

 

Agilent technologies

Thermo Fisher Scientific

IZASA

SUPELCO (part of Sigma-Aldrich)

Enantiosep

Konich-Tech

Bruker

 

 

Other companies 

 

Novozymes Spain S.A.

Bioiberica S.A.