Plants Animals Bacteria Fungi Food Authenticity

ISEAC-‐38 | 17-‐20 June 2014, EPFL, Lausanne Scientific Program | General time schedule MONDAY JUNE 16 2014 Time Reception Hall 17.00 -‐ Symposium Registration and Welcome reception 19.00 TUESDAY JUNE 17 2014 08:00-‐09:00 Environmental / Food Registration 09:00 09:10 Opening Ceremony ROOM B (level 0) Environmental Analytical Challenges 09:15 -‐ Integrated electrochemical sensor 09:15 -‐ 09:45 probes for autonomous in situ 09:45 mapping of inorgannic chemical compounds Marie-‐Lou Tercier-‐Waeber 09:45 -‐ PORPHYRINS IN SENSING 09:45 -‐ 10:05 APPLICATIONS 10:05 E. Fagadar-‐Cosma, D. Vlascici, R. Cristescu and G. Fagadar-‐Cosma

10:05 -‐ 10:25

HPLC-‐ICP-‐AES BASED METHODO-‐ LOGY FOR CADMIUM SPECIATION IN FLOATING MACROPHYTES T.E. Romanova and O.V. Shuvaeva

10:05 -‐ 10:25

Reception Hall

ROOM C (level 1) Food Contaminants & Residues Studies on the extractability of incurred pesticides using Quechers Michelangelo Anastassiades ANALYSES OF HONEY BY QUECHERS-‐LC/GC-‐MS-‐MS: DETECTION OF INSECTICIDES (NEONICOTINOIDS, PYRE-‐THROIDS AND PYRAZOLES), AND IMPLICA-‐ TIONS FOR BEE COLLAPSES AND FOR FOOD SAFETY J.M. Bonmatin, D. Paradis, G. Bérail and L.P. Belzunces ANALYSIS OF MIGRATING COMPOUNDS FROM PLASTIC BABY BOTTLES WITH GC-‐MS, GC-‐(Q)TOF MS AND LC-‐QTOF MS M. Onghena, E. Van Hoeck, J. Van Loco, M. Ibáñez, L. Cherta, T. Portolés, E. Pitarch, F. Hernandéz and A. Covaci

38th International symposium on environmental analytical chemistry 3

10:25 -‐ 10:45

10:45 -‐ 11:05 11:05 -‐ 11:35

11:35 -‐ 11:55

11:55 -‐ 12:15

12:15 -‐ 12:35

A NOVEL MICROFLUIDIC DEVICE FOR FAST EXTRAC-‐TION OF POLYCYCLIC AROMATIC HYDROCARBONS (PAHs) FROM ENVIRONMEN-‐TAL WATERS ʹ COMPARISON WITH STIR-‐BAR SORPTIVE EXTRACTION (SBSE) L. Foan, S. Vignoud, F. Ricoul and G. Marchand Coffee break Nanotechnology versus Nanotoxico-‐logy: Controversial Aspects of Nanotechnological Applications Harald Krug FIELD-‐FLOW FRACTIONATION USING ROTATING COILED COLUMNS IN THE ANALYSIS OF ENVIRONMENTAL PARTICULATE SAMPLES P.S. Fedotov, M.S. Ermolin and O.N. Katasonova A NOVEL METHOD FOR DIRECT DETECTION OF SILVER NANOPARTICLES IN SOLID SAMPLES K. Leopold and N. Feichtmeier

10:25 -‐ 10:45

SIMULTANEOUS DETERMINA-‐TION OF HIGHLY POLAR PESTICIDEs in fRUITS AND VEGETABLES by LC-‐ MS/MS C. Díez, A. Staub Sporri, E. Cognard, D. Ortelli, P. Edder and S. Rudaz

10:45 -‐ 11:05 11:05 -‐ 11:35

Coffee break

11:35 -‐ 11:55

ACCELERATED DISCOVERY AND PROFILING OF PHARMACOLOGICALLY ACTIVE FOOD -‐ INTRODUCING A NOVEL WORKFLOW FOR FOODOMICS. G. E. Morlock and I. Klingelhoefer

11:55 -‐ 12:15

ANALYSIS OF PRIMARY AMINES FROM NYLON FOOD UTENSILS BY LIQUID CHRO-‐MATOGRAPHY-‐ ORBITRAP HIGH RESOLUTION MASS SPECTROMETRY Y. Sanchis, C. Coscollà, and V. Yusà TARGETED SCREENING AND QUANTIFICATION OF PCB AND DIOXINS IN VARIOUS FOODSTUFFS BY PTV LARGE VOLUME INJECTION COUPLED TO GC-‐MS/MS D. Ortelli, N. H. Ho, A. Bugey, P. Zimmerli, J. Nançoz, and P. Edder

DEVELOPMENT OF A NEW METHOD 12:15 -‐ FOR ON-‐SITE MERCURY EXTRAC-‐ 12:35 TION FROM WATERS BASED ON GOLD NANOPARTICLE ADSORBERS J. Huber, M. Schlathauer and K. Leopold

Advances in Rapid Testing Techno-‐ logies for Food Safety and Quality Assessment Franz Ulberth

Lunch break

38th International symposium on environmental analytical chemistry

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ISEAC-‐38 | 17-‐20 June 2014, EPFL, Lausanne Scientific Program | General time schedule

14:00 -‐ 14:20

14:20 -‐ 14:50

14:50 -‐ 15:10

15:10 -‐ 15:30

15:30 -‐ 15:50

Sponsor scientific talk Susanne Feifel Büchi Laboratory, Product Group Manager, Kjeldahl, Dumas and Extraction Solutions From dirt to data ʹ overcome the bottleneck in everyday simple preparation tasks using BUCHI solutions Sampling

14:00 -‐ 14:20

Sponsor scientific talk Christian Hummert, Director AGRI and CTS Food, SGS Germany  Trends in quality management for food ʹ a service provider perspective

Understanding phytoplankton community dynamics using in situ high-‐resolution automated monitoring Francesco Pomati DEVELOPMENT OF A PASSIVE SAMPLER FOR THE QUANTIFICA-‐ TION OF INORGA-‐NIC MERCURY AND METHYLMERCURY IN FRESHWATERS A. Magnier, A. Dabrin, G. Grisot and M. Coquery FIBER-‐OPTIC CHEMIFLUO-‐RESCENT IMMUNOASSAY FOR CONTINUOUS MONITORING OF AIRBORNE MITE ALLERGEN DER F1 K. Miyajima, Y. Suzuki, D. Miki, M. Arai, K. Toma, T. Arakawa, H. Shimomura and K. Mitsubayashi MULTI-‐RESIDUE ANALYSIS OF EMERGING POLLUTANTS IN BEN-‐ THIC INVERTEBRATES BY MODIFIED MICRO-‐QUECHERS EXTRACTION AND NANOLC-‐ MS/MS ANALYSIS: A NEW STRATEGY TO EVALUATE BIOACCUMULATION A. Berlioz-‐Barbier, A. Buleté, E. Vulliet and C. Cren

14:20 -‐ 14:40

Food Authenticity 1: Genomics and Proteomics FOODOMICS ʹ PROTEIN / PEPTIDE BIOACTIVES AND THEIR HEALTH EFFECTS M. Kussmann, A. Panchaud and Michael Affolter PICOSECOND INFRARED LASER (PIRL) AS A NOVEL TOOL FOR BIOMOLECULE EXTRACTION M. Wurlitzer, M. Kwiatkowski, L. Ren, R.J.D. Miller and H. Schlüter

14:40 -‐ 15:00

15:00 -‐ 15:30

Ultrabarcoding: current applications and future potential of genomic technology for high resolution identification of biological materials Quentin Cronk

15:30 -‐ 15:50

DNA-‐BASED FOOD AUTHENTI-‐CITY CONTROL BY CLASSICAL AS WELL AS ISOTHERMAL AMPLIFICATION METHODS AND NEXT GENERATION SEQUENCING I. Haase, T. Janke, K. Juling, C. Käppel, R. Schubbert and S. Schulz


15:50 -‐ 16:10

POPULATION NORMALIZATION WITH AMMONIUM (NH4-‐N) IN WASTEWATER-‐BASED EPIDEMILOGY F. Been, L. Rossi, C. Ort, S. Rudaz, O. Delémont and P. Esseiva Exhibition & Poster session

15:50 -‐ 16:10

APPLYING POPULATION GENETICS FOR AUTHENTIFI-‐CATION OF MARINE FISH K. Behrmann, M. Fischer and H. Rehbein

16:10 -‐ 18:00 18:00 -‐ Social event 19:30 Tasting of vaudois wines WEDNESDAY JUNE 18 2014 ROOM B (level 0) Environmental ROOM C (level 1) Food Multi screening methods Food Authenticity 2: Metabolomics 09:00 -‐ Contaminant diversity of the 09:00 -‐ New insights into Food Quality 09:30 aquatic environment 09:30 Control by NMR Based Screening Heinz Singer Manfred Spraul 09:30 -‐ A MULTI-‐RESIDUE METHOD FOR 09:30 -‐ VALIDATION OF 1H NMR METHODS 09:50 ANALYSIS OF VARIOUS ENDOCRINE 09:50 FOR JUICE AND WINE ANALYSIS DISRUPTORS IN INDOOR AND Y. B. Monakhova, B. Schütz, H. OUTDOOR AIR Schäfer, M. Spraul, T. Kuballa, R. E. Moreau-‐Guigon, F. Alliot, J. Godelmann, H. Hahn and Gasperi, M.J. Teil, M. Blanchard, D. W. Lachenmeier C. Mandin and M. Chevreuil 09:50 -‐ IMPLEMENTATION OF COMPLE-‐ 09:50 -‐ FOOD ANALYSIS TO CHECK 10:10 MENTARY MONITO-‐RING 10:10 QUALITY, SAFETY AND STRATEGIES FOR AN EFFECTIVE-‐ AUTHENTICITY BY FULL-‐ SURVEY OF PSYCHOTROPIC DRUGS AUTOMATED 1H-‐NMR AND METABOLITES IN DRINKING M. Link, M. Spraul, H. Schaefer, WATER TREATMENT PLANTS IN THE F. Fang and B. Schuetz PARISIAN AREA G. Lavison-‐Bompard, S. Lardy-‐ Fontan, V.Brieudes, P. Candido, M. Joyeux, B. Lalere and H. Budzinski 10:10 -‐ SCREENING TOWARDS PHARMA-‐ 10:10 -‐ FOOD PROFILING: AUTHENTICITY 10:30 CEUTICAL RESIDUES IN WASTE-‐ 10:30 CONTROL BY UPLC-‐ESI-‐UHR-‐QTOF WATER BASED ON ACCURATE MASS MASS SPECTROMETRY AND ISOTOPIC PATTERN USING P. Werner and M. Fischer HIGH-‐RESOLUTION ORBITRAP MASS SPECTROMETRY th 38 International symposium on environmental analytical chemistry

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ISEAC-‐38 | 17-‐20 June 2014, EPFL, Lausanne Scientific Program | General time schedule

10:30 -‐ 10:50 10:50 -‐ 11:20

11:20 -‐ 12:40 Lunch break 14:00 -‐ 14:30 14:30 -‐ 14:50 14:50 -‐ 15:10 15:10 -‐ 15:30 15:40 -‐ 16:00

16.00 -‐ 16:20 16:20 -‐ 16:40 16:45 -‐ 18:00

19:15 -‐ 23:30

L. Vergeynst, H. Van Langenhove and K. Demeestere Coffee break Development of passive samplers for a better assessment of the chemical water quality: application to pesticides and pharmaceutical compounds Hélène Budzinski Poster talks

09:30 -‐ 10:50 10:50 -‐ 11:20

Coffee break

11:20 -‐ 12:40

Poster talks

OMICS approaches in food safety: from research tool to routine diagnostic Martin Wiedmann

ROOM B (level 0) Environmental & Food Emerging technologies for environment & food analytics 1 Tracking food with stable isotopes in practice Markus Boner SIMPLE AND INEXPENSIVE METHOD FOR ANALYSIS OF LIQUID SAMPLES S. Pihlasalo, Å. Rinnan, N. Kiskonen, N. Hollo, J. Nurmi, P. Hänninen and H. Härmä ELEMENTAL PROFILING BY ICP-‐AES COMBINED WITH SEPARATION AND CHEMOMETRIC TOOLS IN BOTANICAL ORIGIN DETERMINATION S. ZŽŶēĞǀŝđ, >͘WŝƚĂƌĞǀŝđ^ǀĞĚƌƵǎŝđ͕/͘ Nemet, T. Hudina ĂŶĚ͘Dŝƚŝđ IMPROVING THE COMPARABILITY OF ANALYTICAL ENVIRONMENTAL MEASUREMENTS BY THE IMPLEMENTATION OF A METROLOGICAL INFRASTRUCTURE J. Cabillic TRANSFORMATION OF DRUGS OF ABUSE DURING WATER CHLORINATION: A LIQUID CHROMATOGRAPHY-‐QUADRUPOLE-‐TIME-‐ OF-‐FLIGHT-‐MASS SPECTROMETRY ASSESSMENT J.B. Quintana, I. González-‐Mariño, I. Rodríguez and R. Cela DEDICATED REFERENCE MATERIALS AS A N ESSENTIAL TOOL FOR QUALITY CONTROL IN ENVIRONMENTAL RESEARCH (project MODAS) M. Rutkowska, K. Dubalska, P. Konieczka and J. EĂŵŝĞƑŶŝŬ Coffee break Public lecture Title: Science meets public Subtitle: Food Safety: Simple Goals -‐ Complicated Realities Steven Musser, Deputy Center Director for Scientific Operations, Center for Food Safety and Applied Nutrition, Food & Drug Administration (FDA, USA) Social event Gala dinner during a cruise on the lake Geneva 38th International symposium on environmental analytical chemistry 7

THURSDAY JUNE 19 2014 10:00 -‐ Think Tank -‐ Food safety in a global market: Challenges for authorities, food industry 12:30 and analytical strategies Anchorman: Prof. Dr. Ulrich Noehle (Germany) Participants: ELKE ANKLAM, PhD, European Commission, Directorate General Joint Research Centre, Institute for Reference Materials and Measurements (Belgium) MICHAEL BEER, Director Food Safety Division, Federal Office of Public Health (Switzerland) ANTHONY HUGGETT, Head Corporate Quality Management, Nestlé (Switzerland) CHRISTIAN HUMMERT, Ph.D., Director AGRI and CTS Food, SGS Germany (Germany) STEVEN MUSSER, Ph.D., FDA (Food & Drug Administration), Deputy Center Director for Scientific Operations, Center for Food Safety and Applied Nutrition, FDA (USA) SILVIO RAGGINI, Head Quality Management, COOP (Switzerland) REINER WITTKOWSKI, Ph.D, Prof., Vice President, BfR (Federal Institute for Risk Assessment) BfR (Germany) Lunch break Emerging technologies for environment & food analytics 2 14:00 -‐ Safety of food packaging materials from a food manufacturer perspective: Integrating 14:30 analytical chemistry, biological activity (computational) toxicology and risk assessment. Amaury Patin 14:30 -‐ CHEMICAL ANALYSIS AND RISK ASSESSMENT OF PHTHALATES IN FOODS 14:50 M. Kim, J.-‐M. Oh, H.-‐S. Lim and J.-‐C. Choi 14:50 -‐ HOTMELTS: ADHESION WITH RISK OF CONTAMINATION? 15:10 M. Lommatzsch, T. Simat, M. Biedermann and K. Grob 15:10 -‐ Coffee break 15:30 15:30 -‐ Emerging technologies in mid-‐infrared sensing for environmental and food analysis 16:00 Boris Mizaikoff 16:00 -‐ MERCURY SPECIATION IN URBAN DUST AFFECTED BY GOLD MINING ʹ 16:20 CHARACTERISATION, MODELLING, AND ASSESSMENT OF BIOAVAILABILITY E.M. Cukrowska, J. Lusilao-‐Makiese Julien, B. Yalala, H. Tutu and L.K. Chimuka 16:20 -‐ DEVELOPMENT OF A NEW PASSIVE SAMPLER BASED ON DIFFUSIVE MILLI-‐GEL BEADS 16:40 FOR THE MEASUREMENT OF LABILE COPPER IN VINEYARD SOIL M. Perez, S. Reynaud, G. Lespes, M. Potin-‐Gautier, E. Mignard, P. Chéry,


8

ISEAC-‐38 | 17-‐20 June 2014, EPFL, Lausanne Scientific Program | General time schedule D. Schaumlöffel and B. Grassl R. Frei Awards

16:40 -‐ 17:15 17:30 -‐ IAEAC General Assembly 18:25 Open to everybody, right of vote only for IAEAC members FRIDAY JUNE 20 2014 ROOM B (level 0) Environmental & Food Emerging technologies for environment & food analytics 2 09:00 -‐ Microfluidic nanofiber-‐based biosensor systems 09:30 Baeumner, A.J. 09:30 -‐ APTAMERS: NOVEL APPLICATIONS FOR FOOD ANALYSIS 09:50 T. Huenniger and M. Fischer 09:50 -‐ RAPID AND SELECTIVE BACTERIA DETECTION USING CONDUCTIVE POLYMER FILMS 10:10 S. Tokonami, H. Nakata, M. Ikemoto, T. Kadoma, S. Takami, H. Shiigi and T. Nagaoka 10:10 -‐ ELECTROCHEMICAL BIOSENSORS FOR ENVIRONMENT AND FOOD SAFETY 10:30 J. Rishpon, M. Buch, A. Nassar, O. Sela and M. Mossberg 10:30 ʹ Coffee break 10:50 10:50 ʹ BIOMONITORING SURVEY OF RESIDENTS AND EMERGENCY RESPONDERS EXPOSED TO 11:10 ACRYLONITRILE AFTER THE TRAIN DISASTER IN WETTEREN (BELGIUM) J. Van Loco, T. De Smedt, K. De Cremer, S. Fierens, C. Vleminckx, I. Van Overmeire, G. Gijs, A. Van Nieuwenhuyse and H. Van Oyen 11:10 -‐ ARSENIC, ANTIMONY AND CHROMIUM SPECIATION USING HPLC-‐ICP-‐MS TECHNIQUE IN 11:30 SELECTED RIVERS ECOSYSTEMS OF UPPER SILESIA, POLAND ʹ VALIDATION OF METHODOLOGY M. Jablonska-‐Czapla 11:30 -‐ d,/^KWZK:d͞d,E/>^W/&/d/KE&KZd,h^K&dyZ&/E/K>K'/>E 11:50 Es/ZKEDEd>E>z^/^͟ A. Gross, L.E. Depero, L. Borgese, K. Tsuji, T. Yamada, E. Margui and C. Streli 11:50 -‐ Closing ceremony 12:30


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Dear participants, We are very happy to welcome you to Lausanne for the 38th International symposium on environmental analytical chemistry and food safety (ISEAC 38). ISEAC conferences are a series of bi-annual meetings organized by the International Association of Environmental Analytical Chemistry (IAEAC). This year, for the first time, half of the conference addresses the field of food safety. We are covering classical topics like the analysis of contaminants and residues as well as novel approaches towards authenticity control by emerging technologies based on DNA, proteins, metabolites and elements. Food safety is not only a matter of health protection and environmental quality. Food Safety is affected by a complex network of many stakeholders, economic groups and individuals. The complexity of the food chain is becoming more and more interdisciplinary and global. How can we assure food safety by the interplay of authorities, industry and last but not least by institutions that are responsible for education and teaching all over the world? Do we need novel and innovative strategies to ensure safe food or to overcome food fraud? Are there demands for new analytical approaches to assure product identification and food traceability? The International Think Tank on Food Safety is an integral part of ISEAC38 bringing together leading food safety experts from Europe and USA to approach and discuss food safety globally. It provides the opportunity to learn about food safety along the whole food supply chain in a global context. And, seeing the interest of the participants, this seems to be the way to follow in the future. It is the second time that EPFL accommodate these series of symposia, now in the beautiful new Swiss Tech Convention Center. We hope that you will enjoy the very exciting program prepared by our Scientific Committee that you can discover in the next pages. Don't miss the public lecture “Science meets public” Food Safety: Simple Goals – Complicated Realities, Wednesday end of afternoon; and the Think Tank on Food safety in a global market, Thursday morning. And don't forget the marvelous gala dinner on a boat sailing on the Lake Geneva. On behalf of the Scientific and organizing committees and the IAEAC, we wish you a successful and scientific stimulating symposium in our beautiful region of Lake Geneva. If you have the opportunity, we encourage you to visit our region, its beautiful landscape (Lavaux UNESCO Heritage), cultural attractions and the Olympic Museum. Dr. Luiz F. de Alencastro Prof. Markus Fisher

38th International symposium on environmental analytical chemistry !

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Welcome! To the 38th International Symposium on Environmental Analytical Chemistry (ISEAC) in Lausanne I welcome you on behalf of the International Association of Environmental Analytical Chemistry (IAEAC), the organization behind this ISEAC 38. The IAEAC is a more than 40 years young non-profit organization under Swiss Law, who aims at fostering progress in the field of the analytical sciences with reference to the Environment in the broadest sense. The ISEAC is held biannually and brings together researchers and users of analytical methodology, manufacturers of analytical instrumentation and industry as well as government laboratories using the methodology and instrumentation to as solve complex analytical tasks in the field of chemical analysis in the environment in the most broadest sense. This year a special emphasis is food quality in all its aspects. This meeting including an exhibition, lectures, posters and a think tank on food safety with internationally acting leaders in the field is held in the new Swiss Tech Convention Center at the EPFL campus in Lausanne. We look all forward for a stimulating meeting with ample opportunities for networking on an interdisciplinary basis. For the International Association for Environmental Analytical Chemistry Prof. Dr. José A.C. Broekaert, President

It is a great honour for EPFL to host the 38th edition of the International Symposium on Environmental Analytical Chemistry in our new SwissTech Convention Center. As far back as 1986 EPFL had the privilege to organize this important conference, demonstrating a long term interest and investment in environmental chemistry. Those of you who participated 28 years ago might not recognize the campus: EPFL has tripled its student population reaching 10’000 students this year! For the first time in its history, this year’s edition of IAEAC includes a session and a Think Tank on Food Safety. This topic is of particular interest for EPFL, with research ongoing in this domain in our Institute of Environmental Engineering, in the Schools of Life Sciences, Basic Sciences and Engineering, and in the Nestlé Institute of Health Sciences situated in EPFL’s Innovation Park. Our modern society is facing major challenges in terms of food safety and the development of novel analytic methods, based on chemical, molecular and genetic approaches, is essential to assure the quality of food and prevent fraud. We wish you a stimulating conference at EPFL. We hope that you have time to explore our campus and that the SwissTech Convention Center will provide an inspiring backdrop for new thoughts and innovative scientific contributions. Patrick Aebischer, President of EPFL 38th International symposium on environmental analytical chemistry ! ! !

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Committees Honorary Committee! Mauro Dell’Ambrogio, State Secretary for Education, Research and Innovation, Berne! Jacqueline de Quattro, Head of the Department for Security and Environment, Canton de Vaud !Daniel Brélaz, Mayor of the City of Lausanne! Patrick Aebischer, President, EPF, Lausanne! Josef Tremp, Head Industrial Chemicals Section, Federal Office for the Environment-FOEN, Berne! Andrea Rinaldo, Professor, EPF, Lausanne! Paul Joseph Dyson, Professor, EPF, Lausanne! Vera Slaveykova, Professor, University of Genevè! Hans Jörg Bachmann, President of the Swiss Society for Food and Environmental Chemistry, Berne Scientific Committee Luiz Felippe de Alencastro, EPF, Lausanne – co-chairman Markus Fischer, University of Hamburg – co-chairman Antje Baeumner, Cornell University Eric Bakker, University of Geneva José A.C. Broekaert, University of Hamburg – President IAEAC Patrick Edder, SCAV, Food and Veterinary Control Authority of Geneva Pierre Esseiva, University of Lausanne Montserrat Filella, University of Geneva Thomas Gude, Swiss quality testing services (SQTS), Dietikon Tamar Kohn, EPF, Lausanne Urs Von Gunten, EPF, Lausanne / EAWAG, Dübendorf Lionel Spack, Nestlé Research Center, Lausanne Richard Stadler, Nestlé, Quality Assurance Center, Vevey Markus Zennegg, Swiss Federal Laboratories for Materials Science & Technology, EMPA, Dübendorf Local Organizing Committee Felippe de Alencastro, EPF, Lausanne – co-chairman Joseph Tarradellas, EPF, Lausanne Sonja Desplos, Symposium coordination – IAEAC, Lausanne


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EO16 IMPLEMENTATION OF COMPLEMENTARY MONITORING STRATEGIES FOR AN EFFECTIVESURVEY OF PSYCHOTROPIC DRUGS AND METABOLITES IN DRINKING WATER TREATMENT PLANTS IN THE PARISIAN AREA G. Lavison-Bompard1, S. Lardy-Fontan2, V.Brieudes2,3, P. Candido1, M. Joyeux1, B. Lalere1, H. Budzinski3 1

DRDQE, Eau de Paris, 33 avenue Jean Jaurès, 94 200 Ivry sur Seine, France.

2

Laboratoire National de métrologie et d’Essais (LNE), 1 rue Gaston Boissier, 75724 Paris, France.

3

ISM-LPTC, UMR 5255, CNRS-Université Bordeaux 1, 351 cours de la Libération, 33405 Talence,

France.

Through the last decades, ubiquitous contamination of water, all through its cycle, by pharmaceuticals residues has been demonstrated. More recently, the scope of attention has been widening to psychotropic drugs. According to this recent interest, this work presents the survey of 68 French’ relevant psychotropic compounds -including 29 metabolites and glucuronides of a broad range of benzodiazepines, hypnotic drugs, antidepressants, stimulants, opiates and opioids, anticonvulsants, anti-dementia drugs as well as anthropic tracers. Two complementary sampling approaches were simultaneously implemented on two drinking water treatment plants (influent and effluent) located nearby Paris. The first approach was based on grab sampling and the second on passive sampling using polar organic compound integrative samplers (POCIS). Those last enable to concentrate in situ trace pollutants and yields in time-weighted averaged concentrations. Main results, advantages and limits of the implemented strategy as well as lessons will be presented and discussed.


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EO17 SCREENING TOWARDS PHARMACEUTICAL RESIDUES IN WASTEWATER BASED ON ACCURATE MASS AND ISOTOPIC PATTERN USING HIGH-RESOLUTION ORBITRAP MASS SPECTROMETRY L. Vergeynst, H. Van Langenhove, K. Demeestere Ghent University, Department of Sustainable Organic Chemistry and Technology, Research Group EnVOC, Coupure Links 653, 9000 Ghent, Belgium

Modern high-resolution mass spectrometry (HRMS) such as Orbitrap technology coupled to ultra-high performance liquid chromatography (UHPLC) enables full-scan analysis of a virtually unlimited number of (emerging) organic contaminants in water at trace levels. This raises the opportunity for post-acquisition suspect screening, but obtaining acceptable low false negative and false positive rates is still challenging. In this study, a novel screening strategy is elaborated for 40 suspect pharmaceuticals in wastewater using a fully validated analytical method based on Orbitrap HRMS. Both the accurate mass (error) of the mono isotopic ion and up to three isotopes and their isotope ratios are considered as multiple variates of a statistical model. A powerful screening strategy, able to automatically detect peaks (centWave algorithm) and to match isotopes, is developed guarantying a false negative rate of 5%. Preliminary results show a false positive rate (false positive count / number of suspect compounds) decreasing drastically from 183, 49, 9 to 2% when taking only the isotopic ion, 1, 2 and 3 isotopes into account, respectively. Incorporating a peak/noise filter further reduced the false positive rate to 74, 33, 6 and 2%, respectively, without compromising the false negative rate. In conclusion, despite the lower abundance of isotopes, which might compromise the detection limits, the novel screening approach using isotopes and a peak/noise filter clearly improves the identification success rate.


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EO18 DEVELOPMENT OF PASSIVE SAMPLERS FOR A BETTER ASSESSMENT OF THE CHEMICAL WATER QUALITY : APPLICATION TO PESTICIDES AND PHARMACEUTICAL COMPOUNDS Budzinski Helene, Belles Angel, Cruz Justine, Dufour Vincent, Tapie Nathalie University of Bordeaux, EPOC-LPTC, UMR 5805 CNRS, 351 crs de la Liberation, 33405 Talence cedex, France The European legislation, and in particular the Water Frame Work Directive (WFD) requires the development of cost efficient monitoring tools that can provide the required information for the assessment of water contamination. Passive sampling methods are ones of the new interesting tools that have a potential to be used in various regulatory monitoring programmes aimed at assessing the levels of chemical pollutants. The performance and benefits of passive sampling approach are now commonly recognized. For example, the SPMD (Semi Permeable Membrane Device) has been widely documented. It allows to asses the water dissolved hydrophobic pollutant concentrations. Moreover those methods are particularly interesting for sampling polar compounds in water because they take into account the temporal variability and integrate the pollutant contamination over the whole sampler deployment period. Recently considerable effort has been directed towards the development of passive sampling methods that are suitable for the monitoring of polar organic compounds that are found commonly in water bodies. Two passive samplers have been reported that are suitable for monitoring of a broad range of polar compounds in water: Chemcatcher and POCIS (Polar Organic Chemical Integrative Samplers) (Togola et Budzinski, Mazzella et al, 2008, Gunold et al, 2007). Concerning these polar compounds like pharmaceuticals and pesticides, the most used tool for their sampling is POCIS, which needs more development to improve its quantitative aspect. Indeed, the performance and the sampling rates of target compounds are not the same between the laboratory and the environment because sampling rates are influenced by a range of environmental factors such as temperature, hydrodynamic conditions…. Moreover, the membrane contribution to mass transfer of pollutants into the receiving phase can be significant and could act as a barrier for the accumulation into the tool. In this study, the POCIS were optimized for pharmaceuticals and pesticides in various laboratory experiments. In order to improve the quantitative aspect, the Performance Reference Compound approach (PRC) (PRCs are compounds introduced into the receiving phase prior to exposure) was developed for POCIS. Various PRCs were tested under several conditions. These laboratory improvements were then applied to the Gironde estuary and Arcachon Bay (France) where all studied compounds were monitored during one year. The results showed a spatial and seasonal variability of the dissipation rates of PRC. The results suggest that the environmental conditions affect the POCIS performance over the season and the sampling site. Considering the PRC dissipation, the compound water concentrations were easily calculated. Moreover, an adaptation of POCIS was proposed using Nylon membranes. This adaptation has allowed to improve sensitivity and also in some cases to decrease the so-called “lag-effect’ improving the quantitative aspect of the tool. Acknowledgments: Région Aquitaine, CPER A2E (Région Aquitaine and FEDER), ANR RIPOST, FEDER Zostere n° 32953 and ANR EMESTOX (ANR PRECODD 2008) are acknowledged for financial support. 38th International symposium on environmental analytical chemistry !

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EO19

ELEMENTAL PROFILING BY ICP-AES COMBINED WITH SEPARATION AND CHEMOMETRIC TOOLS IN BOTANICAL ORIGIN DETERMINATION

S. Ron!evi"1, L. Pitarevi" Svedru#i"1, I. Nemet1, T. Hudina2, B. Miti"2 1

Laboratory of Analytical Chemistry, Department of Chemistry, Faculty of Science,

University of Zagreb, Horvatovac 102 a, 10000 Zagreb, Croatia 2

Department of Botany and Botanical Garden, Division of Biology, Faculty of Science, University of

Zagreb, Maruli"ev trg 9a, 10000 Zagreb, Croatia !

Characterization of elemental content is basic requirement in quality analysis of food and herbal products as well as in botanical and geographical origin postulations. Inductively coupled plasma source with optical detection (ICP-AES) shows an exclusive advantage in “elemental profiling” due to highly sensitive simultaneous multielement analysis with high precision, large dynamic range and low detection limits. Analytical approaches in fingerprinting which rely on combination of different analytical techniques and with aid of chemometrics is remarkably useful in standardization of food and herbal products as well as in chemotaxonomy of plants. The results of combined analytical methods are presented by two examples. The first includes pollen analysis and multielement analysis of honey samples from Northwestern counties of Croatia. The chemometric interpretation of results provides valuable information regarding quality, authenticity and botanical origin of Croatian continental honey. The second example describes combination of elemental analysis of pyrethrum plant varieties and HPLC separation of natural insecticide extracts of pyrethrins. By applying the multivariate statistical tools some specific assignments of wild and cultivated varieties were established. The information integrated from the inorganic constituents’ level and natural insecticide content provides valuable results for the plant chemotaxonomy purposes.


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EO20

TRANSFORMATION OF DRUGS OF ABUSE DURING WATER CHLORINATION: A LIQUID CHROMATOGRAPHY-QUADRUPOLE-TIME-OF-FLIGHT-MASS SPECTROMETRY ASSESSMENT

J.B. Quintana, I. González-Mariño, I. Rodríguez, R. Cela Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, Constantino Candeira SN, 15782-Santiago de Compostela, Spain.

Illicit drugs and their metabolites are continuously released into surface waters by sewage treatment plant effluents. Aside from the potential impact on the aquatic environment, their presence in rivers and lakes might imply negative consequences for humans if these water resources are used for drinking water production. On that basis, this presentation compiles the transformation underwent by some of the most frequently abused illicit drugs during water chlorination, the commonest disinfection process worldwide. Experiments were performed at laboratory scale, spiking individual samples with one particular compound and analyzing different reaction times aliquots by liquid chromatography-quadrupole-time-of-flight-mass spectrometry (LC-QTOF-MS). Factors affecting the degradation process were studied in detail by experimental designs, and kinetics equations were established in every case. Transformation products were firstly identified by single MS analyses and, subsequently, their structures were elucidated by interpreting their fragmentation patterns in the MS/MS product ion scan mode. Finally, the chlorination process was studied with real surface waters in order to evaluate the extent of the reaction and to verify the formation of by-products. Acknowledgements: Spanish MINECO (project no. CTQ2010-18927 and CTQ2012-33080), Galician Government (postdoctoral grant to I.G. M.) and FEDER funds.


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EO21 DEDICATED REFERENCE MATERIALS AS AN ESSENTIAL TOOL FOR QUALITY CONTROL IN ENVIRONMENTAL RESEARCH (project MODAS)

Ma"gorzata Rutkowska, Kinga Dubalska, Piotr Konieczka, Jacek Namie#nik Department of Analytical Chemistry, Faculty of Chemistry, Gda$sk University of Technology, 80-233 Gda$sk, 11/12 G. Narutowicza Street, Poland

Reference materials are an essential element of the system control and quality assurance measurements. The demand for analytical information on the composition of various material objects makes it necessary for the production of an even wider range of reference materials. Although the number of reference materials commercially available continues to grow there are still areas such environmental analysis where their absence is felt. In 2012 started the implementation of tasks within the project MODAS. Final results of this work will be obtain a "package" six certified reference materials, which can be regarded as a response to the needs of Polish analytical laboratories in the field of broader environmental analysis. Four of them (bottom sediment, herring tissue, codfish tissue, cormorant tissue) select characteristic for trophic chain of Polish marine ecosystem. These materials will be characterized by both the diversity of the composition of the matrix as well as a wide range of analytes. The most important feature of the production is to be representative of the composition of both the matrix and the levels of analytes in comparison to typical environmental samples tested in the Polish analytical laboratories. Development, production and implementation of the practice of analytical reference materials is the process laborious, time-consuming and expensive. The presentation shows a general scheme of the proceedings leading to the preparation of reference material as well as problems and challenges present at every stage of the production process, on the basis of the results of determination of total mercury in each of the materials. Manufactured in certified reference materials after completion of the project will form the sample used in research aimed at the validation of analytical laboratories and Polish will be an important complement to the current offer of certified reference materials available on the market/field.


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EO22

EMERGING TECHNOLOGIES IN MID-INFRARED SENSING FOR ENVIRONMENTAL AND FOOD ANALYSIS

Boris Mizaikoff, University of Ulm, Institute of Analytical and Bioanalytical Chemistry, 89081 Ulm, Germany --- uni-ulm.de/iabc --- [email protected]

State-of-the-art sensing platforms ideally benefit from miniaturized and integrated optical technologies providing direct access to molecule-specific information. With in-situ sensing strategies e.g., in harsh environments or point-of-care diagnostics in medicine becoming more prevalent, detection schemes that do not require reagents or labeled constituents facilitate localized on-site analysis close to realtime. However, decreasing the analytically probed volume may adversely affect the associated analytical figures of merit such as the signal-to-noise-ratio, the representativeness of the sample, or the fidelity of the obtained analytical signal. Consequently, the guiding paradigm for the miniaturization of optical diagnostic devices should be creating chem/bio sensing platforms that are as small as still useful, rather than as small as possible, and that smartly capitalize on advantageous features of integrated photonics. Mid-infrared (MIR; 3-20 $m) sensor technology is increasingly adopted in environmental analysis, process monitoring and biodiagnostics, as well as food analysis and food safety, due to the inherent molecular specificity enabling the discrimination of molecular constituents at ppm-ppb concentration levels in condensed and vapor phase media. Recently emerging strategies taking advantage of innovative waveguide technologies such as mid-infrared transparent fiberoptics, substrate-integrated hollow waveguides, and planar semiconductor waveguides (e.g., MIR Mach-Zehnder interferometers) in combination with highly efficient light sources such as broadly tunable quantum cascade lasers facilitate compact yet robust MIR diagnostic platforms for label-free chem/bio sensing and diagnostics. 38th International symposium on environmental analytical chemistry !

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EO23 MERCURY SPECIATION IN URBAN DUST AFFECTED BY GOLD MINING – CHARACTERISATION, MODELLING, AND ASSESSMENT OF BIOAVAILABILITY E.M. Cukrowska, J. Lusilao-Makiese Julien, B. Yalala, H. Tutu, and L.K. Chimuka University of the Witwatersrand, Environmental Analytical Chemistry, MSI Smit Street 1, PO Box 3 WITS, 2050 Johannesburg, South Africa

The growing global concern over the mercury pollution has prompted specific inventories that quantify mercury emissions from various sources. To assess human expose to mercury in urban areas, the inhalable dust should be included in a study. The Witwatersrand Basin in South Africa is one of the most important mining regions in the world. Mercury, which occurs in gold-bearing ores, was also used for gold recoveries till 1920 and presently in illegal artisanal mining. The city of Johannesburg is a multimillion population. The aim of this study was to determine the mercury pollution in this area and assess its bioavailability from inhalable dust. Dust samples were collected at inhalation levels and separated into fractions. Mercury concentrations were determined by CVAFS. The results showed that HgTOT ranged from 300 to 1700 µg kg-1 for PM 25 particle size fraction with extremely high concentrations in industrial areas, especially around reprocessed gold tailings, above 100 000 µgkg-1. Bioavailability of mercury from inhalable dust was assessed by leaching fractions of dust samples with artificial lung fluids (the upper and the lower lungs. Oral bioavailability was evaluated using the artificial gastric juice and hydrochloric acid. The leaching conditions were set up to mimic lungs and stomach environment. Leaching showed that most of the mercury inhaled with dust is extracted in the deep interstitial parts of the lungs. The artificial gastric juice (AGJ) leached out 2% Hg. BCR sequential extraction procedure also showed the predominance of non-soluble Hg species (90–98%) in studied dust samples.


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EO24 DEVELOPMENT OF A NEW PASSIVE SAMPLER BASED ON DIFFUSIVE MILLI-GEL BEADS FOR THE MEASUREMENT OF LABILE COPPER IN VINEYARD SOIL M. Pereza, S. Reynauda, G. Lespesa, M. Potin-Gautiera, E. Mignardb, P. Chéryc, D. Schaumlöffela, B. Grassla a

Université de Pau et des Pays de l'Adour (UPPA)/CNRS, Laboratoire de Chimie Analytique BioInorganique et Environnement, UMR IPREM 5254-Technopôle Hélioparc, Av. du Président Angot, 64053 Pau Cedex, France b CNRS-Solvay-Universit!é Bordeaux, UMR5258, Laboratoire du Futur, 178 Avenue du Dr. A. Schweitzer, 33608 Pessac Cedex, France c Bordeaux Science Agro, 1 cours du Général De Gaulle, Gradignan, 33175, France

In viticulture, the use of Bordeaux mixture containing copper can fight effectively against downy mildew caused by a fungal pathogen. Repeated use of this fungicide during years has resulted in an accumulation of copper in vineyard soils. The aim of this study was to develop a reliable analytical tool for the measurement of labile copper in soil for environmental management of this element. For this, a strategy based on the use of innovative passive samplers has been implemented. After exposure of the samplers to copper, an elution step followed by Inductively Coupled Plasma! Atomic Emission Spectrometry (ICP-AES) allowed the analysis of the concentration of this element retained by the sampler. Based on the same principle as diffusive gradient in thin-films (DGT), these novel samplers are made of a Diffusive Milli-Gel (DMG) which consists of a hydrogel nanocomposite and a chelating resin able to absorb the bioavailable portion of copper. They differ from classic samplers by their unique geometry as a result of the manufacturing technique. A droplet-flow millifluidic process allowed precise control of the size and the geometry of each DMG bead. The synthesis by this process provided a system composed of several spherical DMG beads of around 1 millimeter diameter. The main advantage of this device is the increase of the exchange surface improving the analysis of the targeted chemical element. DMGs are composed of a polyacrylamide gel crosslinked in which a cation exchange resin is incorporated. A set of experiments highlighted two important parameters for the control of the resin inclusion: the particle size of the resin and the flow rates used for the synthesis by the millifluidic technique. This technique offers the possibility to synthetize a range of passive samplers with various concentrations of polymer, crosslinking agent and chelating resin which potentially allow a high adaptability of the system to the type of soil or to the presumed metal concentration. DMG opens a lot of perspectives and opportunities in environmental monitoring as in situ technique for dynamic trace metal partition. The first in situ monitoring measurements of copper solution using DMG will be presented. 38th International symposium on environmental analytical chemistry !

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EO25 MICROFLUIDIC NANOFIBER-BASED SYSTEMS FOR SAMPLE PREPARATION

Baeumner, A.J.1, 2, Matloc-Colangelo, L.2, Georgescu, A.1,2, Frey, M.W.3 1

Institute of Analytical Chemistry, Chemo- and Biosensors, University of Regensburg,

Universitaetsstr. 31, Regensburg, Germany 2

Department of Biological and Environmental Engineering, Cornell University, Ithaca, NY, USA

3

Department of Fiber Science and Apparel Design, Cornell University, Ithaca, NY, USA

Microfluidic biosensors, labs-on-a-chip and lateral flow assays for the detection of viable organisms, toxins, and clinically relevant markers have been successfully developed in our research group including analytes such as B. anthracis, C. parvum, dengue virus, E. coli, S. pyogenes, cholera toxin, CD4+ T-lymphocytes, thrombin and myoglobin. Recently, we initiated the study of electrospun nanofibers and their potential to enhance bioassays in paper-based lateral-flow assays (LFA) and in polymer-based microfluidic devices by adding functionalities to the formats otherwise not available. In the case of the LFA format we successfully demonstrated the de novo fabrication of nanofiber-mats as membrane material enabling immobilization of biorecognition elements, adding novel surface chemistries and preventing nonspecific binding without the use of blocking reagents. Nanofiber-enhanced microfluidic devices provide additional degrees of freedom for bioassay designs, as nanofibers with various surface chemistries are electrospun into distinct locations in the microfluidic channels. As the resulting fiber mats can be of varying density and size and hence generate a 3D-structure within the channels intimate contact with the sample is guaranteed throughout the channel volume. Current investigations study these systems for sample preparation, as mixers, and as concentrators where, for example, a concentration of E. coli cells by a factor of 20,000 has already been demonstrated. We also develop a nanofiber modelling software that enables fluid dynamic studies to investigate mixing capabilities within our microfluidic devices. 38th International symposium on environmental analytical chemistry !

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EO26 RAPID AND SELECTIVE BACTERIA DETECTION USING CONDUCTIVE POLYMER FILMS

S. Tokonami1, H. Nakata1, M. Ikemoto1, T. Kadoma2, S. Takami2, H. Shiigi3, T. Nagaoka3 1

Nanoscience and Nanotechnology Research Center, Research Organization for the 21st Century,

Osaka Prefecture University, 1-2 Gakuen-cho, Sakai 599-8570, Japan 2

Sharp Corporation, 3-1-72, Kitakamei-cho, Yao 581-8585, Japan

3

Department of Applied Chemistry, Graduate School of Engineering, Osaka Prefecture University, 1-2

Gakuen-cho, Sakai 599-8570, Japan

A bacterial surface-structure transferred polypyrrole film was successfully developed for the rapid and specific recognition of bacteria. In general, bacteria are classified into two groups: Gram-negative and Gram-positive, according to the chemical structure of their surfaces. Regardless of their surface chemical structures, both were doped on a polypyrrole film vertically as long as they were negatively charged. The doped bacteria were successfully removed by electrochemical oxidation of the film, creating shape-complementary cavities to the template bacteria. The unique technical combination of the film with dielectrophoresis made the specific detection of template bacteria possible at concentrations as low as 103 CFU/mL within 3 min, without any bacterial pretreatment. Furthermore, the bacterial cavities had high selectivity and were able to discriminate particular target bacteria, P. aeruginosa, out of bacterial mixtures containing A. calcoaceticus, E. coli, and S. marcescens.


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EO27 BIOMONITORING SURVEY OF RESIDENTS AND EMERGENCY RESPONDERS EXPOSED TO ACRYLONITRILE AFTER THE TRAIN DISASTER IN WETTEREN (BELGIUM) J. Van Loco1, T. De Smedt2, K. De Cremer1, S. Fierens2, C. Vleminckx2, I. Van Overmeire1, G. Gijs3, A. Van Nieuwenhuyse2 & H. Van Oyen2 1

Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Brussels, Belgium

2

Public Health & Surveillance, Scientific Institute of Public Health, Brussels, Belgium

3

Health care & crisis management, FPS Health, Food chain safety and Environment, Brussels,

Belgium On Mai 4, 2013, a train transporting chemicals derailed in Wetteren (Belgium). Wagons with the toxic acrylonitrile (ACN,) exploded. ACN has been classified as possibly carcinogenic to humans (Group 2B). During the disaster, ACN was dissolved with water used to fight the fire and flowed into the sewers. The population and emergency responders were exposed via toxic fumes to ACN and its decomposition product cyanide coming out of the sewers or from the fire. One person died, around 200 persons were hospitalized, around 2000 residents were evacuated and approximately 2000 emergency responders were deployed. To assess the exposure of the local population and the emergency responders, a biomonitoring study was setup. ACN exposure was assessed by analyzing as biomarker the N-2-cyanoethylvaline (CEV) in haemoglobin. Since smoking is a confounder, cotinine analysis was also performed. Of the 242 participating residents, 33% of the non-smokers have CEV adduct concentrations above the reference value of 10 pmol/g globin and among the smokers, 47% have CEV adduct concentrations above the reference value for smokers of 200 pmol/g globin. The distribution pattern of the CEV adduct concentrations above the reference value indicate that exposure in the residents follows the sewer network. 1053 emergency responders participated, and 23% of the non-smokers have CEV concentrations above the reference value while for the 28% of the smokers their CEV levels are above the 200 pmol/globin. 38th International symposium on environmental analytical chemistry !

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EO28 ARSENIC,

ANTIMONY

AND

CHROMIUM

SPECIATION

USING

HPLC-ICP-MS

TECHNIQUE IN SELECTED RIVERS ECOSYSTEMS OF UPPER SILESIA, POLAND – VALIDATION OF METHODOLOGY M. Jab%o&ska-Czapla Institute of Environmental Engineering of the Polish Academy of Sciences, M. Sk%odowskiej-Curie Str. 34, 41-819 Zabrze, Poland The results of toxicological tests show that (in many cases) it is not the total content of a given element but its various forms that have a decisive impact on the living organisms. A classic example of such diverse properties are such ions as Cr(III) and Cr(VI) Sb (III), Sb(V) and arsenic speciation forms: As(III), As(V), MMA, DMA, AB. The aim of this study was to optimize and validate methods for determination of these ions using HPLC-ICP-MS system and their application to study the content of these analytes in highly polluted river ecosystems of Upper Silesia (K%odnica, Bytomka, Bia%a Przemsza, Rawa). Separation step was done on high-performance liquid chromatograph equipped with ion-exchange column followed by ICP-MS spectrometer detector. In this study the validation process was applied to all stages of sample preparation and analysis (selection of the calibration curve, determination the method sensitivity, accuracy and precision, quantification and detection limit obtaining, identification of analyte recovery, estimation of method selectivity). The work is a part of the MoSpeSil project (2013-2015) supported by Small Grant Scheme 2012 the Polish-Norwegian Research Programme.


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EO30 THE ISO PROJECT “TECHNICAL SPECIFIATION FOR THE USE OF TXRF IN BIOLOGICAL AND ENVIRONMENTAL ANALYSIS” A. Gross1, L.E. Depero2, L. Borgese2, K. Tsuji3, T. Yamada4, E. Margui5and C. Streli6 1

Bruker Nano GmbH, Berlin, Germany;

2

University of Brescia, Chemistry for Technologies Laboratory, Brescia, Italy;

3

Graduate School of Engineering, Osaka City University, Osaka, Japan;

4

Rigaku Corporation, Takatsuki, Osaka, Japan;

5

Department of Chemistry, University of Girona, Girona, Spain;

6

TU Wien, Atominstitut, Radiation physics, Vienna, Austria

Total reflection X-Ray Fluorescence spectroscopy (TXRF) today is a powerful multielemental method for trace and ultratrace analysis of different kind of samples that can be grouped as follows: environmental samples (as water, soil, aerosols, deposits, plants), geological and mineralogical samples (as ore, crystals, mineral raw materials), biological samples (as blood, serum, urine, human tissue), food samples (as fish, fruit, meat, nuts, mushroom) and many others. Presently, two international standards for the contamination analysis on silicon wafers by TXRF exist, but none for the chemical analysis of the beforehand listed sample groups. Recently, a workgroup at the ISO Technical committee 201 started a project “Technical Specifiation for the use of TXRF in biological and environmental analysis” (WD 18507). The objective for the document is to provide a framework on the uses of Total reflection X-Ray Fluorescence (TXRF) for biological and environmental elemental qualitative and quantitative analysis of elements. It is meant to help technicians, biologist, environmental scientists, and engineers to understand the possible uses of TXRF for elemental analysis by providing the guidelines for the characterization of biological and environmental samples with TXRF spectroscopy. This paper explains results of a first round robin test on water samples and provides an update about the working draft of the technical specification and an outlook about future TXRF projects of the ISO workgroup. 38th International symposium on environmental analytical chemistry !

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EO31 IMPROVING THE COMPARABILITY OF ANALYTICAL ENVIRONMENTAL MEASUREMENTS BY THE IMPLEMENTATION OF A METROLOGICAL INFRASTRUCTURE J. Cabillic, C. Fallot, B. Lalere and S. Vaslin Reimann LNE - Biomedical and Organic Chemistry Department, 1 rue gaston Boissier, 75724 Paris 15, France

Surveillance, prevention and protection of the environment has become a major issue and the major concerns of citizens national and international public policy. All of the decision systems are based on the data, that is the reason why a considerable weight is placed on the quality of the measurement. The quality of the measurement implies that we need reliable measurements (trueness and precision) and comparable (traceable and with a level of known and mastered uncertainty). It is then important to be sure that methods implemented by routine laboratories fulfilled those quality criterias. The two main tools used to control the quality of the data are: - reference materials: there is few reference materials for organic compounds in the field of environment mainly due to stability problems of those compounds. But they are very important to make the quality of laboratories’ data reliable by providing a reference value at concentration and uncertainty levels required by the legislation, - inter laboratories comparisons (ILC): performance evaluations is mainly doing by participation in ILC which reference value is a consensus value. This value is not traceable to the International System (SI). There is a strong need to connect these reference values to a primary reference method. Through different practical examples relating to the analysis of Polycyclic Aromatic Hydrocarbon in representative matrix (water, air…), the work will present the development of reference materials and reference methods to assess reference value during ILC.


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EO32 DETERMINATION OF HIGHLY POLAR COMPOUNDS IN FOOD BY LC-MS/MS C. Díez*1,2, A. Staub Sporri1, E. Cognard1, D. Ortelli1, P. Edder1 and S. Rudaz2 1

: Official Food Authority Control and Veterinary Affairs (SCAV). Quai Ernest-Ansermet 22, 1211 Geneva (Switzerland) 2 : School of Pharmaceutical Sciences - University of Lausanne, University of Geneva, 20, Bd d'Yvoy, 1211 Geneva (Switzerland)

The determination of problematic highly polar compounds (antibiotics and pesticides) not usually covered by routine multiresidue methods was discussed in this study. For their analysis, the nature of the stationary phase (liquid separation cell and hydrophilic interaction chromatography with different supports), mobile phase (water or buffer solutions with acetonitrile), pH, gradient conditions and injection solvents were studied as relevant parameters for tuning retention and selectivity by LCMS/MS. Adequate sensitivity, good peak shape and resolution were achieved by the use of Obelisc R with 1% formic acid as mobile phase for aminoglycosides and with an acidified formate buffer mobile phase for highly polar pesticides. An extraction procedure for honey and kidney proposed by Kumar et al. (J. Sep. Scie. 2012) was adapted for the analysis of aminoglycosides in animal derived products with a polymeric weak cation exchange cartridge. The final method was validated according to Commission Decision 2002/657/EC. Highly polar pesticides were extracted from fruits and vegetables with an acidified methanol extraction. Important signal suppression due to matrix effect was observed in this case and different clean-up techniques were evaluated with the aim of enhancing their sensitivity.


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FOOD SAFETY

LECTURES !


"#!

OF1 OF2

Michelangelo Anastassiades, CVUA Stuttgart, Fellbach, Germany !"#$%&!'()'"*&'&+",-."-/%0%"1'(2'%).#,,&$'3&!"%.%$&!'#!%)4'56&.7&,!' ' J.M. Bonmatin, CNRS, Centre de Biophysique Moléculaire, Orléans Cedex 02, France. ANALYSES OF HONEY BY QUECHERS-LC/GC-MS-MS: DETECTION OF INSECTICIDES (NEONICOTINOIDS, PYRETHROIDS AND PYRAZOLES), AND IMPLICATIONS FOR BEE COLLAPSES AND FOR FOOD SAFETY

OF3

M. Onghena, Toxicological Center, Department of Pharmaceutical Sciences, University of Antwerp, Wilrijk-Antwerp, Belgium ANALYSIS OF MIGRATING COMPOUNDS FROM PLASTIC BABY BOTTLES WITH GCMS, GC-(Q)TOF MS AND LC-QTOF MS

OF4

C. Diez, Official Food Authority Control and Veterinary Affairs (SCAV) and School of Pharmaceutical Sciences - University of Lausanne, University of Geneva, Geneva, Switzerland SIMULTANEOUS DETERMINATION OF HIGHLY POLAR PESTICIDES IN FRUITS AND VEGETABLES BY LC-MS/MS

OF5

Franz Ulberth, Euopean Commission, DG Joint Research Centre, Institute for Reference Materials and Measurements, Geel, Belgium ADVANCES IN RAPID TESTING TECHNOLOGIES FOR FOOD SAFETY AND QUALITY ASSESSMENT

OF6

G.E. Morlock, Justus Liebig University Giessen, Chair of Food Science, Interdisciplinary Research Center, Giessen, Germany ACCELERATED DISCOVERY AND PROFILING OF PHARMACOLOGICALLY ACTIVE FOOD - INTRODUCING A NOVEL WORKFLOW FOR FOODOMICS

OF7

Yovana Sanchis, Foundation for the Promotion of the Health and Biomedical Research in the Valencia Region (FISABIO-Public Health) and Public Health Laboratory of Valencia, Spain ANALYSIS OF PRIMARY AMINES FROM NYLON FOOD UTENSILS BY LIQUID CHROMATOGRAPHY-ORBITRAP HIGH RESOLUTION MASS SPECTROMETRY

OF8

D. Ortelli, Official Food Control Authority of Geneva, Switzerland TARGETED SCREENING AND QUANTIFICATION OF PCB AND DIOXINS IN VARIOUS FOODSTUFFS BY PTV LARGE VOLUME INJECTION COUPLED TO GC-MS/MS

OF9

Martin Kussmann, Molecular Biomarkers, Nestlé Institute of Health Sciences (NIHS), Lausanne, Switzerland. Faculty of Life Sciences, Ecole Polytechnique Fédérale Lausanne (EPFL), Switzerland and Faculty of Science, Interdisc. NanoScience Center (iNANO), Aarhus University, Danemark. FOODOMICS - PROTEIN/PEPTIDE BIOACTIVES AND THEIR HEALTH EFFECTS

OF10

Wurlitzer M., Massenspektrometrische Proteom-Analytik, Institut für Klinische Chemie & Laboratoriumsmedizin, Campus Forschung, Hamburg, Germany PICOSECOND INFRARED LASER (PIRL) AS A NOVEL TOOL FOR BIOMOLECULE EXTRACTION


69

OF11

Quentin Cronk, Dept of Botany and Beaty Biodiversity Research Centre, University of British Columbia, Vancouver, Canada ULTRABARCODING: CURRENT APPLICATIONS AND FUTURE POTENTIAL OF GENOMIC TECHNOLOGY FOR HIGH RESOLUTION IDENTIFICATION OF BIOLOGICAL MATERIALS

OF12

I. Haase, Eurofins Genomics, Anzingerstr. 7a, 85560 Ebersberg, Germany DNA-BASED FOOD AUTHENTICITY CONTROL BY CLASSICAL AS WELL AS ISOTHERMAL AMPLIFICATION METHODS AND NEXT GENERATION SEQUENCING

OF13

K. Behrmann, University of Hamburg - Hamburg School of Food Science Hamburg and Max Rubner-Institut (MRI), Federal Research Institute for Nutrition and Food, Dept of Safety and Quality of Milk and Fish products, Hamburg, Germany APPLYING POPULATION GENETICS FOR AUTHENTIFICATION OF MARINE FISH

OF14

M. Spraul, Bruker BioSpin GmbH, Rheinstetten, Germany NEW INSIGHTS INTO FOOD QUALITY CONTROL BY NMR BASED SCREENING

OF15

Y. B. Monakhova, Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe and Bruker Biospin GmbH, Silbersteifen, Rheinstetten, Germany VALIDATION OF 1H NMR METHODS FOR JUICE AND WINE ANALYSIS

OF16

M. Link, Bruker BioSpin GmbH, Business Development, Rheinstetten, Germany FOOD ANALYSIS TO CHECK QUALITY, SAFETY AND AUTHENTICITY BY FULLAUTOMATED 1H-NMR

OF17

Werner P., Hamburg School of Food Sciences; Institute of Food Chemistry, University of Hamburg, Germany FOOD PROFILING: AUTHENTICITY CONTROL BY UPLC-ESI-UHR-QTOF MASS SPECTROMETRY

OF18

Martin Wiedmann, Dept of Food Science, Cornell University, Ithaca, NY, USA OMICS APPROACHES IN FOOD SAFETY: FROM RESEARCH TOOL TO ROUTINE DIAGNOSTIC

OF19

Markus Boner, Agroisolab GmbH, Jülich, Germany TRACKING FOOD WITH STABLE ISOTOPES IN PRACTICE

OF20

S. Pihlasalo, University of Turku, Laboratory of Biophysics, Turku, Finland SIMPLE AND INEXPENSIVE METHOD FOR ANALYSIS OF LIQUID SAMPLES

OF21

S. Ron!evic, Lab. of Analytical Chemistry, Department of Chemistry, Faculty of Science, University of Zagreb, Zagreb, Croatia ELEMENTAL PROFILING BY ICP-AES COMBINED WITH SEPARATION AND CHEMOMETRIC TOOLS IN BOTANICAL ORIGIN DETERMINATION

OF22

Dr Steven Musser, Deputy Center Director for Scientific Operations, Center for Food Safety and Applied Nutrition, Food & Drug Administration (FDA), College Park, USA Science meets public FOOD SAFETY : SIMPLE GOALS ! COMPLICATED REALITIES


70

OF23

Yves-Alexis Hammel, Nestlé Research Center, Lausanne, Switzerland SAFETY OF FOOD PACKAGING MATERIALS FROM A FOOD MANUFACTURER PERSPECTIVE: INTEGRATING ANALYTICAL CHEMISTRY, BIOLOGICAL ACTIVITY (COMPUTATIONAL) TOXICOLOGY AND RISK ASSESSMENT

OF24

Meehye Kim, Food additives and Packaging Division, Ministry of Food and Drug Safety, Osong, Korea CHEMICAL ANALYSIS AND RISK ASSESSMENT OF PHTHALATES IN FOODS

OF25

M. Lommatzsch, Kantonales Labor Zurich, GC Department, Zurich, Switzerland

HOTMELTS: ADHESION WITH RISK OF CONTAMINATION? OF26 Hünniger T., Hamburg School of Food Science; Institute of Food Chemistry, University of Hamburg, Germany APTAMERS: NOVEL APPLICATIONS FOR FOOD ANALYSIS OF27 J. Rishpon, Tel-Aviv University, Department of Molecular Microbiology and Biotechnology, Ramat-Aviv, Israel ELECTROCHEMICAL BIOSENSORS FOR ENVIRONMENT AND FOOD SAFETY


71

OF1 STUDIES ON THE EXTRACTABILITY OF INCURRED PESTICIDES USING QuEChERS Michelangelo Anastassiades, Julia Hepperle, Daniela Roux, Anja Barth EU-Reference Laboratory for Pesticide Residues requiring Single Residue Methods hosted at: CVUA Stuttgart, Schaflandstrasse 3/2, D-70736 Fellbach E-Mail: [email protected]

10 years following its first publication QuEChERS has evolved to the most widely used method for pesticide residue control worldwide. Although QuEChERS provides excellent recoveries of a broad range of spiked pesticides, special attention is necessary when extracting incurred pesticides. This presentation deals with the impact of various factors on the extraction yields of incurred pesticides such as solvent, temperature, agitation approach and particle size. Extraction time and temperature were shown to have the most substantial impact on the extraction yields of incurred pesticides whereas agitation intensity seems to play a less significant role. Pesticide yields from samples employed frozen reached a “plateau” after ca.10-15 min compared to ca. 2 minutes when employed at room temperature. The use of mechanical shakers is recommended. The extraction yields were further shown to strongly depend on the physiochemical properties of the pesticides. Lipophilic pesticides show the strongest retardation and therefore also the highest yield-increases when extraction times and/or temperature are increased. The impact of prolonging extraction time from 1 to 15 min, on the extraction yields from frozen samples was studied on 132 real crop samples containing 85 different pesticides of a broad polarity range. Out of the 408 pesticide/commodity combinations studied 34% showed >25% yield-increase when prolonging extraction to 15 min. More than half of the 132 tested samples contained at least one pesticide showing >25% yield increase. Similar extraction retardation effects were also observed for spiked pesticides but only if spiked on commodities with intact surface, not to homogenates thereof.


73

!"#$ ANALYSES OF HONEY BY QUECHERS-LC/GC-MS-MS: DETECTION OF INSECTICIDES (NEONICOTINOIDS, PYRETHROIDS AND PYRAZOLES), AND IMPLICATIONS FOR BEE COLLAPSES AND FOR FOOD SAFETY J.M. Bonmatin*1, D. Paradis2, G. Bérail2 and L.P. Belzunces3 1

CNRS, Centre de Biophysique Moléculaire, 45071 Orléans Cedex 02, France.

2

LEAV, Rond-point Georges Duval, 85021 La Roche sur Yon Cedex, France.

3

INRA, Lab. de Toxicologie Environnementale, 84914 Avignon Cedex 9, France.

We developed a single extraction process, followed by two separation-detection methods depending on the pesticides of interest. This analytical protocol was tested with various types of honey (nectars and honey; mono-floral and multi-floral). These 2 methods were validated for 25 major insecticides. Analyses were performed after a QuEChERS type extraction, starting from 5 g of honey, then by using GC-MS-MS for the pyrazoles and pyrethroids or LC-MS-MS for the nicotinoids. Selectivity, linearity, reproducibility were statistically checked. Mean extraction yields were between 80% and 130%. The 2 methods were validated with a LOQ at 0.5 ng/g for all the insecticides. Honey bees and bumble bees are very sensitive to insecticides. They play an essential role in pollination of plants and are also efficient bioindicators of agricultural pollution. New systemic pesticides are highly suspected to participate to the bee collapse of pollinators observed worldwide. Our analytical methods were required to detect these relevant pesticides in hive products, with a high sensitivity (LOD quite below the ng/g level). Concerning food safety, honey is largely consumed worldwide. Our analytical methods developed for honey, can be easily applied for various matrices such as fruits, cereals, or vegetables. !

!


74

OF3 ANALYSIS OF MIGRATING COMPOUNDS FROM PLASTIC BABY BOTTLES WITH GCMS, GC-(Q)TOF MS AND LC-QTOF MS M. Onghena(a), E. Van Hoeck(b), J. Van Loco(b), M. Ibáñez(c), L. Cherta(c), T. Portolés(c), E. Pitarch(c), F. Hernandéz(c), A. Covaci(a) (a) Toxicological Center, Department of Pharmaceutical Sciences, University of Antwerp, Universiteitsplein 1, B-2610 Wilrijk-Antwerp, Belgium (b) Scientific Institute of Public Health (WIV-ISP), J. Wytsmanstraat 14, B-1050 Brussels, Belgium (c) Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain Bisphenol-A (BPA), a monomer for polycarbonate polymers (water and infant feeding bottles) and epoxy resins (canned food packaging), can be released into the food and so contaminate people. Since BPA has endocrine disrupting properties, its use was recently prohibited for the production of polymers for food contact materials for children younger than 3 years old (European Commission, regulation (EU) N° 10/2011). Consequently, alternatives to polycarbonate food contact materials for children, such as polypropylene, polyethersulfone, polyamide, Tritan® or silicone baby bottles, have appeared on the market. The principal aim of our study was the identification of major compounds migrating from these baby bottles. In this context, the use of simulants is prescribed in the legislation to mimic the testing of real foods. Specifically, we selected a mixture of water:EtOH (50:50) as a simulant for milk. After sterilization of the bottle during ten minutes with boiling water, three migrations were performed during 2h at 70 °C. A non-targeted liquid-liquid extraction method with ethyl acetate:n-hexane (1:1), previously optimized with a mixture of 17 commonly migrating organic compounds, was performed on the simulant samples. The extracts were first analyzed by GC-MS followed by an untargeted database search using Wiley® and NIST® libraries. Various compounds, such as alkanes, phthalates, amides, fatty acids, antioxidants, etc. were detected. Unidentified peaks were further investigated by GC-(EI)-TOF MS and GC-(APCI)-QTOF MS to specifically elucidate the structure of these unknown compounds. The expected presence of the accurate mass molecular ion and/or protonated molecule in APCI together with the fragmentation pattern observed in both techniques mentioned above were used for elucidation purposes. Additionally, extracts were analysed also by LC-QTOF MS under MSE mode. The full-spectrum accurate mass data of both (de)protonated molecule and fragment ions were acquired simultaneously. Data were automatically processed using a home-made database containing around 1200 contaminants based on the PIM ((EU) N° 10/2011) and expected migrating compounds such as anti-oxidants, plasticizers, etc. When a peak was detected, and its reference standard was not available at our lab, a tentative identification was performed using the accurate mass of the observed fragment ions. Several compounds which were previously not identified by GC-MS analysis were detected. Although generally the concentrations of these migrating compounds were relatively low (ng/g to µg/g range), additional toxicological research needs to be done to evaluate the potential risk of all these migrants for human health. !

!


75

OF4 SIMULTANEOUS DETERMINATION OF HIGHLY POLAR PESTICIDES IN FRUITS AND VEGETABLES BY LC-MS/MS C. Díez*1,2, A. Staub Sporri1, E. Cognard1, D. Ortelli1, P. Edder1 and S. Rudaz2 1

: Official Food Authority Control and Veterinary Affairs (SCAV). Quai Ernest-Ansermet 22, 1211

Geneva (Switzerland) 2

: School of Pharmaceutical Sciences - University of Lausanne, University of Geneva, 20, Bd d'Yvoy,

1211 Geneva (Switzerland)

Several highly polar pesticides, most of them belonging to the ammonium quaternary family, were selected for this study. Their analysis by Obelisc R stationary phase (liquid separation cell technology) was evaluated. The nature of the mobile phase (water or buffer solutions with acetonitrile), pH (percentage of formic acid), gradient conditions and injection solvents were studied as relevant parameters for tuning retention and selectivity of these highly polar pesticides by LC-MS/MS. Adequate sensitivity, good peak shape and resolution were achieved with an acidified formate buffer mobile phase. An acidified methanol extraction for fruits and vegetables was carried out but important signal suppression was observed due to matrix effect. Different sorbents (PSA, C18, GCB, weak cation exchange) in dispersive solid-phase extraction mode were studied with the aim of enhancing the pesticide detection. The final method was validated according to Document SANCO No. 12571/2013 and provided limits of quantitation below the established maximum residue levels within the European and Swiss legislations.

*

: Corresponding author: e-mail: [email protected]; Tel: +41(0)225465972; Fax:

+41(0)225465696 38th International symposium on environmental analytical chemistry

76

OF5 ADVANCES IN RAPID TESTING TECHNOLOGIES FOR FOOD SAFETY AND QUALITY ASSESSMENT Franz Ulberth, Euopean Commission, DG Joint Research Centre, Institute for Reference Materials and Measurements, Retieseweg 111, 2440 Geel, Belgium Email : "#$%&'()*+#,-.+/'+(#01$'+( The free movement of safe and wholesome food is an essential aspect of the internal market and contributes significantly to the health and well-being of EU citizens and to their social and economic interests. Due to globalization and the availability of new technological processes the European food and feed sector is becoming more and more complex. In the past several food scares have shattered the trust consumers have in their food supply. To restore confidence a complex regulatory framework has been set up in the EU. Maximum limits for a diverse array of undesirable substances in the food chain have been laid down, appropriate sampling and analysis methods for official control purposes have been described, and a rapid warning and response system has been introduced. Control activities have to be risk based in order to direct limited resources to areas of high importance for public health. Rapid methods, often also called screening methods, offer the possibility to screen a large number of test items for the presence of a hazardous agent; more laborious testing procedures are then applied to confirm their presence or to determine accurately the amount present. Another useful application of rapid methods could be their use in acceptance sampling plans, where, depending on the sampling plan, a substantial number of individual laboratory samples have to be tested to determine whether to accept or reject a lot. Screening methods, as any other testing methodology for official food control, need to be validated, preferably by collaborative study. Several suggestions for a study protocol for qualitative tests exist; however, harmonization is still necessary. Examples for screening methods and their validation will be given in the presentation.


77

OF6 ACCELERATED DISCOVERY AND PROFILING OF PHARMACOLOGICALLY ACTIVE FOOD - INTRODUCING A NOVEL WORKFLOW FOR FOODOMICS

G.E. Morlock and I. Klingelhoefer Justus Liebig University Giessen, Chair of Food Science, Interdisciplinary Research Center (IFZ), Heinrich-Buff-Ring 26-32, 35392 Giessen, Germany !

Food and food supplements can be unknowingly pharmacologically active. Traditional medicines are supposed to be bioactive, although the active principle is unclear. Complex samples like food contain thousands of single compounds. Only known target compounds are looked for, however, most bioactive compounds in food are unknown. On the contrary, untargeted analyses face the challenge of determining the thousand peaks’ identities, but it remains largely unclear which peaks are bioactive. Here we show a novel effect-directed food profiling. By effect-directed microorganisms, all bioactive compounds in food were quantitatively detected as sharp-bounded zones, characterized by mass spectrometry. This workflow can be used in personalized health care and contributes with fast answers to patients’ susceptibilities to disease or their responses to traditional medicines, and to tailor their nutrition and lifestyle management accordingly. It allows frequent food intakes to be identified as risky with regard to special diseases, giving fundamental insights into food-borne pathogenesis.


78

OF7 ANALYSIS OF PRIMARY AMINES FROM NYLON FOOD UTENSILS BY LIQUID CHROMATOGRAPHY-ORBITRAP HIGH RESOLUTION MASS SPECTROMETRY Yovana Sanchis1,2 , Clara Coscollà1,2, and Vicent Yusà1,2,,3* 1

Foundation for the Promotion of the Health and Biomedical Research in the Valencia Region

(FISABIO-Public Health), 21, Avenida Catalunya, 46020 Valencia, Spain 2

Public Health Laboratory of Valencia, 21, Avenida Catalunya, 46020 Valencia, Spain

3

Analytical Chemistry Department, Universit of Valencia, Edifici Jeroni Muñoz,Dr. Moliner 50, 46100

Burjassot, Spain

Primary aromatic amines (PAAs) appear in food products since they are widely used in the textile, food contact materials, agriculture and pharmaceutical industries and evidence suggest that some PAAs are carcinogenic pollutants. A simple and rapid method has been developed for the determination of 8 primary amines (2,6 Toluendiamine, 2,4 Toluendiamine, Aniline, 1,5 Naphthalenediamine, 1,3 Phenylenediamine , 4-4’ diaminodiphenilmetano ,4-4’ Oxidianilina ,otolidine) in nylon utensilies using Liquid Chromatography-Orbitrap High Resolution Mass Spectrometry (UHPLC-Orbitrap-HRMS) working at a resolving power of 50000 FWHM in full scan, with fragmentation mode (HCD) and a high mass accuracy (50% post acidic treatment), and also an increase in the Fe & Ti content. Moreover, SEM analyses indicated several crystallographic changes upon treatment of the ashes (e.g. formation of Ettringite-Thaumasite compounds). It has been demonstrated that the fly ash particle’s crystallographic structure and surface was changed appreciably, which will affect the interactions with transition metal ions. Keywords: fly ash, crystallographic structure, structural changes, matrix SEM, surface chemistry


212

PE101 LOWER LIMITS OF DETECTION THROUGH INCREASED NEBULIZATION EFFICIENCY OF ESI/MS METHOD A. Laanistea, A. Kruvea, A. Saluveea, I. Leitoa, Koit Herodesa, Rünno Lõhmusb,Ants Lõhmusb, Fredrik Pungac

a

University of Tartu, Institute of Chemistry, Ravila 14a, 50411 Tartu

b

University of Tartu, Institute of Physics, Ravila 142, 51014 Tartu

c

Estonian Nanotechnology Competence Centre, Ravila 142, 51014 Tartu

It is increasingly important to be able to analyze smaller amounts of analytes with ESI/MS method and thus ionization strategies with higher efficiency are needed. Our group has introduced a novel nebulizer design (called 3R) with addition of extra gas capillary into the eluent capillary. 3R nebulizer offers lower LoDs than commercial nebulizer due to increased signal-to-noise ratio (about 50 times). For 16 pesticides LoD improvement of 2,5 times on average (highest result 200 times) was observed in case of solvent, garlic, onion and tomato. Lower LoDs were also obtained for neonicotinoids in honey samples (on average 2 times) and linear range reached at lower concentrations with 3R compared to commercial nebulizer. In light of 2-year ban of 3 neonicotinoids (Reg. (EU) No 485/2013) it is increasingly important to be able to determine these at lower concentrations to be able to detect any residue. Nearly 300 honey samples from 2005 – 2013 were analyzed to give an overview of 4 neonicotinoids – thiamethoxam, imidacloprid, acetamiprid, thiacloprid - in Estonian honey. 38% of overall samples contained thiacloprid. Decrease of thiacloprid in honey from 2013 to 2005 was observed, most likely because of stability problems. Highest result observed was 0.14 mg/kg for thiacloprid, which does not exceed MRL 0.2 mg/kg etablished in EU.


213

PE102 ENVIRONMENTAL CHEMISTRY OF TRACE AND ULTRATRACE ELEMENTS

I. Shtangeeva

St. Petersburg University, Chemical Depart, Universitetskaya nab., 7/9, St. Petersburg 199034, Russia

There is a wealth of published experimental material devoted to both essentiality and toxicity of certain trace metals and metalloids. However, the list of the elements is rather short. Until now, little or even no attention has been paid to many of the 90 elements that occur in soil and in different plants. The biological significance of most elements is presently unknown. Moreover, there is a lack of detailed information on concentration of many of these elements in plants. Previously, this was largely due to our inability to accurately detect the minute concentrations of many trace elements in environmental samples. Now there is a unique situation when increasing capability and improving sensitivity of modern analytical methodologies is allowing the rapid development of ultratrace element research. This may serve as a basis for new findings that relate to the environmental chemistry of elements of unknown biological significance. In the paper, we will discuss successful application of several analytical techniques (instrumental neutron activation analysis, ICP-MS and ICP-OES) to determine a wide range of elements in soil and in different plant species grown both in a field and under artificial conditions (green-house and laboratory experiments on modeling of uptake of macro- and trace elements and their transfer within plants). Problems arising during sampling and preparation of environmental samples for elemental analysis as well as application of multivariate statistical methods to the datasets will also be discussed.


214

PE103 MEASUREMENT UNCERTAINTY IN WATER MONITORING: CONTRIBUTION OF BOTH LABORATORYAND

SAMPLING

UNCERTAINTIES.

A

CASE

STUDY

ON

PHARMACEUTICALS IN THE SEINE RIVER (FRANCE)

S. Lardy-Fontan1, G. Lavison-Bompard2, V.Brieudes1,3, P. Candido2, G. Couturier2, B. Lalere1, H. Budzinski3

1

Laboratoire National de métrologie et d’Essais (LNE), 1 rue Gaston Boissier, 75724 Paris, France,

2

DRDQE, Eau de Paris, 33 avenue Jean Jaurès, 94 200 Ivry sur Seine, France.,

3

ISM-LPTC, UMR 5255, CNRS-Université Bordeaux 1, 351 cours de la Libération, 33405 Talence,

France

Overall management and decision making system driven by the Water Framework Directive (WFD) and other European water policies is strongly dependent on monitoring data. As a matter of fact, the need for effective chemical water monitoring is evident as accurate and comparable measurements are sound basis for proper decision making. In that perspective, the present work presents and discusses the estimating of the weight of both laboratory and sampling uncertainty on the overall measurement uncertainties. To do so, two complementary analytical methodologies, held by two laboratories, addressing a set of representative pharmaceuticals were developed and validated with respects to standards on method characterization of performances and uncertainty estimation. Moreover, in order to determine the sampling uncertainty, an experimental design based on the double approach has been designed. It has been successfully implemented on the Seine River (Paris). The proposed work will exhibit and discuss the concepts of bank effects, sampler effects, sampling effects and laboratory effect on the measurement results and uncertainties.


215

PE104 TRIBUTYLTIN QUANTIFICATION BY ISOTOPE DILUTION MASS SPECTROMETRY UNDER THE EUROPEAN WATER FRAMEWORK DIRECTIVE E. Alasonati1, I. Fettig2, B. Fabbri1, C. Yardin1, E. Del Castillo1, P. Panayot3, R. Philipp2, P. Fisicaro1

1

Laboratoire national de métrologie et d'essais (LNE), Biomedical and Inorganic Chemistry Department,

1 rue Gaston Boissier, 75724 Paris, France 2

Bundesanstalt fuer Materialforschung und -pruefung, Richard-Willstaetter-Str. 11, 12489 Berlin,

Germany 3

LGC Limited, Queens Road, Teddington, Middlesex, TW11 0LY, UK

Tributyltin (TBT) is common pollutant of marine and freshwater ecosystems, known to be toxic for living organisms at extremely low levels. In this work primary reference methods capable of quantifying tributyltin at the Environmental Quality Standard (EQS) level imposed by the European Water Framework Directive (WFD) 2000/60/EC in whole water samples, have been developed and validated. The analyses were performed using the isotope dilution (ID) calibration technique and gas chromatography coupled to inductive coupled plasma mass spectrometry (GC-ICP-MS). Different extraction/preconcentration methods have been compared. A design of experiments (DOE) based on a factorial plan has been used to evaluate the solid phase extraction (SPE) approach. Liquid-liquid extraction (LLE) was identified as the method giving the best preconcentration. The procedure has been validated in mineral water at 0.082 ng L-1 (concentration thrice lower than the EQS). The LLE-ID-GCICP-MS approach was transposed to model water which mimics natural surface water with respect to the dissolved organic carbon (DOC) and suspended particulate matter (SPM) content. Moreover, field-flow fractionation (FFF) hyphenated to ICP-MS and jointly speciation analyses in collected fractions were employed to study the partitioning of TBT in water fractions of different sizes and nature.


216

PE105 MEASURING TRACE ELEMENT CONTAMINATION IN SURFACE WATERS USING CHEMICAL AND BIOLOGICAL MONITORING TOOLS

A. Larrose, A. Dabrin, R. Récoura-Massaquant, A. François, J. Gahou, L. Dherret, A. Chaumot, O. Geffard and M. Coquery

Irstea, UR MALY, 5 rue de la Doua, F-69626 Villeurbanne Cedex, France

The measurement of bioavailable trace element fraction is important for environmental assessment. Passive sampling has been suggested as a chemical alternative to biomonitoring. Diffusive Gradient in Thin films (DGT) samplers allow the determination of the ‘labile’ trace element fraction considered to be more representative of the potentially bioavailable fraction than the dissolved fraction. In this study, DGT passive samplers and transplanted organisms (Gammarus fossarum) were deployed in situ to evaluate the trace element contamination of surface waters in 6 watersheds impacted by different anthropogenic activities (agriculture, mixed urban and industrial, mining). Both techniques led to similar conclusion: the maximum pressure of metal contamination occurred in the mining area. In case of intermediate levels of contamination, results were more complex to interpret due to some limitations of the tools: e.g. mechanisms of Cu internal regulation for tested organisms, labile Cd not representing truly bioavailable Cd. Nevertheless, interpretation of the results for elements such as Zn, Co and Ni led to the same classification in term of environmental pressure of contamination: mining > urbanindustrial > vineyard > agricultural. Consequently, this study showed that the tested combination of chemical and biological tools is efficient to assess the pressure of bioavailable trace element contamination at watershed scale.


217

PE106 CHEMICAL COMPOSITION AND UNIQUE CHARACTERISTICS OF SHALLOW ICE CORE SAMPLES FROM A DOME FUJI CORE (ANTARCTICA) DRILLED IN 2001 Yuko Motizuki1, Hideaki Motoyama2, Yoichi Nakai1, Keisuke Suzuki3, Yoshinori Iizuka4, and Kazuya Takahashi1 1

RIKEN Nishina Center, Wako-shi, Saitama 351-0198, Japan National Institute of Polar Research, Midoricho 10-3, Tachikawa 190-8518, Tokyo, Japan 3 Shinshu University, Asahi 3-1-1, Matsumoto 690-8621, Japan 4 Hokkaido University, Kita-ku, Sapporo 060-0808, Japan 2

Ice core samples contain a variety of information of the history of the earth, including climate change in the past. In particular, Dome Fuji, being situated at the highest point of an inner land of East Antarctica, is one of the best drilling locations for procuring to reconstruct past climates and environments. Around this region, several series of ice cores have been obtained and chemical characteristics have been examined (e.g., Kamiyama et al., 1989). We have performed precise measurements of anions and cations for samples from the Dome Fuji ice core drilled in 2001 at depths from 7.7m to 65.0m, corresponding to the ages over the past 1300 years, to investigate the outline of ion balance and its basic geochemical implications. The ice core samples were drilled and cut into pieces around 3-4 cm in length along the depth direction; the temporal resolution corresponds to around 0.9 years. We obtained 1435 samples and the measured anions were HCOO–, CH3COO–, CH3SO3–, F–, Cl–, NO2–, NO3–, SO42–, C2O42–, and PO43–, and the measured cations were Na+, K+, Mg2+, Ca2+, and NH4+, using an ion chromatograph. The concentration level of each ion is from 10 to 300-400 μg/L for most samples. The average of chemical composition is clearly different from that of seawater. Therefore, it is considered that most of the precipitation at Dome Fuji is not subject to sea salts. This confirms the observation by Kamiyama et al. (1989). On the other hand, several peaks have been found in the depth profiles of chloride and sodium ions. For those samples exhibiting chloride and sodium peaks, the concentrations of these two ions correlate with each other and the abundance ratio of sodium to chloride is similar to that of sea salt. This observation indicates that climate conditions were such that precipitation containing sea salt fell in the Dome Fuji area. In those samples in the depth profile not exhibiting Na+ and Cl– peaks, the Na+/Cl– ratio differed from that previously reported for the covering snow. To interpret these observations, further studies, such as isotopic analyses of δD and δ18O, are required. In this presentation, we will show the details of the analyses by ion chromatography and the ion balance.


218

PE107 NOVEL RESINS FOR THE DETERMINATION OF URANIUM BY DIFFUSIVE GRADIENT IN THIN FILMS (DGT) IN URANIUM MINING ENVIRONMENTS J. Drozdzak1, M. Leermakers1, V. Phrommavanh2, M. Descostes2 and W. Baeyens1 1

Vrije Universiteit Brussel VUB, Analytical and Environmental Chemistry Department ANCH,

Pleinlaan 2, Brussels, Belgium 2

AREVA Mines, DEXP/DRD, Tour AREVA, 1 Place Jean Millier, Paris La Défense, France

The application of the technique of Diffusive Gradient in Thin Films (DGT) to water monitoring provides in situ measurement of the time-averaged concentrations of labile metal species in solution. Mining environments are characterized by large variations in pH, ionic strength and concentrations of competing and interfering ions. Thus the resins used must have a high selective binding capacity for uranium and show a good performance under the environmental conditions. Three new resins for uranium, Diphonix resin (Eichrom) and two experimental resins, were investigated and compared with previously used resins for uranium, Chelex®-100 and Metsorb. For the new resins, gel preparation as well as elution procedures were optimized. All resin gels were compared both in lab experiments and at different former mining sites in France. Lab investigation has shown that the three new resins exhibit very good performance across a wide range of pH (i.e. pH 3-9), ionic strength (i.e. 0.001- 0.7 mol L-1 NaNO3). A linearity of U accumulated mass as function of exposure time intervals (2, 6, 10, 24 and 48 h) was demonstrated. Moreover the new resins are characterized by greater U uptake than Chelex®-100 and Metsorb, especially in field conditions, as they are less affected by the nature of the U complexes present.


219

PE108 COMPLEMENTARITY OF LC-MS/MS AND IRMS TO STUDY THE FATE OF ANTIBIOTICS IN SOIL: CASE OF SULFADIMETHOXINE C. Letourniant, R. Baudot, A. Anchisi, M. Batteau, S. Guibert, P. Jame and E. Vulliet Institute for Analytical Sciences, 5 rue de la Doua, 69100 Villeurbanne, France

Sulfonamides are antibiotics which are widely used in many countries to treat human and animal diseases. The widespread occurrence of sulfonamides in all environmental compartments has increased attention over the last few years. Nevertheless, nowadays, only few data are available regarding the fate of sulfonamides in the environment and particularly in soils, mainly by a lack of appropriate analytical methods. This work investigated the complementarily of two analytical methods, namely isotopic ratio analysis (IRMS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) to study the fate of sulfadimethoxine in soil. Experiments were conducted in soil column with

13

C-sulfadimethoxine, in order to better understand

the transfer and transformation of the molecule. Analysis of different soil horizons and leachates were performed simultaneously. The most relevant aspects of the study are reported.


220

PE109a DETERMINATION OF BENZODIAZEPINES IN HOSPITAL WASTEWATER USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY P. Fernández(1), R.A. Lorenzo(2), M.A. Carro(2), M. Regenjo(1). (1) Institute of Forensic Sciences, Forensic Toxicology Service, Faculty of Medicine C/ San Francisco, s/n. 15782-Santiago de Compostela, Spain (2) Department of Analytical Chemistry, Faculty of Chemistry, Avda. de las Ciencias, s/n. 15782-Santiago de Compostela, Spain The benzodiazepines are the psychoactive drugs more prescribed in European countries; so many patients are involved in numerous cases of poisoning due to these drugs. For this reason, the benzodiazepines are considered as emerging environmental pollutants that are commonly found in wastewater. A simple preparation procedure using Ultrasound-assisted-dispersive liquid liquid microextraction (UA-DLLME) was developed for determination of alprazolam, bromazepam, clonazepam, diazepam, lorazepam, lormetazepam and tetrazepam in wastewater from hospital. The benzodiazepines were quantified by ultra performance liquid chromatography with photodiode array detection (UPLC-PDA), using a mobile phase composed of acetonitrile and phosphate buffer pH 6 at a flow of 0.4 mL/min. The method was validated by determining the linearity, selectivity, limits of detection, precision and accuracy. The calibration curves were linear in the range of 0.5-50 ng mL-1. The LOQs of the benzodiazepines were between 0.07 and 0.42 ng mL-1. The analytes recoveries were higher than 80%. Moreover, the precision was acceptable at all concentrations. Finally, the validated method was applied to analyze 30 wastewater samples from hospital, and influents and effluents from six wastewater treatment plants (WWTP). Acknowledgements: This work was supported by the Xunta de Galicia (Projects: 10PXIB208089PR and 10TAL209005PR).


221

PE109b CHROMATOGRAPHIC DETERMINATION OF ANTIDEPRESSANTS IN WASTEWATER

P. Fernández(1), R.A. Lorenzo(2), M.A. Carro(2), M. Regenjo(1).

(1) Institute of Forensic Sciences, Forensic Toxicology Service, Faculty of Medicine C/ San Francisco, s/n. 15782-Santiago de Compostela, Spain (2) Department of Analytical Chemistry. Faculty of Chemistry. Avda. de las Ciencias, s/n. 15782-Santiago de Compostela, Spain

Depression is a serious psychiatric illness and may be fatal since most patients consider suicide. As a result, the prescription of antidepressants and anxiolytics has also increased resulting in a higher incidence of poisoning by these drugs. Due to the high consumption of psychiatric pharmaceuticals and their increasing presence in wastewater, it is necessary to develop new extraction and determination

methods

of

these

substances.

Ultrasound-assisted

dispersive

liquid–liquid

microextraction (UA-DLLME) was optimized for separation determination of escitalopram, fluoxetine, fluvoxamine, mirtazapine, sertraline and venlafaxine from in wastewater. The antidepressants were quantified by ultra performance liquid chromatography with diode array detection (UPLC-PDA), using ACQUITY UPLC® BEH Shield RP18 column (100x2.1mm, 1.7μm particle size) and a mobile phase composed of acetonitrile and phosphate buffer pH 3 at a flow of 0.4 mL/min, in gradient mode, that allows to obtain a good separation of the five compounds in a time of 2 min. The analytical method was validated by determining the linearity, limits of detection, precision, accuracy and recoveries of the target analytes. Acknowledgements: This work was supported by the Xunta de Galicia (Projects: 10PXIB208089PR and 10TAL209005PR).


222

PE110 PREPARATION OF STANDARD VOC MIXTURES FOR CLIMATE MONITORING

A. Demichelis1, G. Sassi1,2 and M. P. Sassi1 1

Istituto Nazionale di Ricerca Metrologica INRIM - Torino, Italy

2

Politecnico di Torino, Dipartimento di Scienza Applicata e Tecnologia - Torino, Italy

European legislation regulates ambient concentrations of VOC key compounds relevant for indoor air monitoring and for air quality and climate monitoring programmes, e.g., the Global Atmosphere Watch (GAW) programme of the WMO. Data Quality Objectives refer to an expanded uncertainty lower than 10% for VOC measurement at concentration lower than 100 nmol/mol. Traceable and accurate standards and standardised dilution methods for VOC concentration are thus essential for the reliability and harmonisation of the measurement data provided. International research projects are ongoing to develop dynamic dilution systems from several sources (static cylinders and dynamic generation) to prepare standards at 1 - 100 nmol/mol VOC concentration with an uncertainty < 2-7 %. The uncertainty sources for VOC mixtures prepared by a single stage dynamic dilutor are here analyzed. Dilution flow rate, purity of the dilution gas, VOC losses and concentration variability due to imperfect gas mixing, wall-adsorption effects and leaks were considered as influence quantities. The dynamic dilutor performance was described by material balances on which a uncertainty budget was redacted. Mixing performances, wall interactions and leak tests were considered to design the dilutor. Design criteria for the dynamic dilutor and design specification for the air purification system were developed. This work contribute to develop standardized dilution methods for a better calibration of monitoring GAW instruments, it will helps to reduce uncertainty in climate change forecasting models.


223

PE111 DETERMINATION OF SAMPLING RATES OF DIFFERENT WATER POLLUTANTS FOR POLAR ORGANIC CHEMICAL INTEGRATIVE SAMPLERS (POCIS) USING A SIMPLE FLOW-THROUGH SYSTEM

S. Tanwar, M. Di Carro and E. Magi

Department of Chemistry and Industrial Chemistry, University of Genoa Via Dodecaneso 31, 16146 Genoa, Italy

Polar Organic Chemical Integrative Sampler (POCIS) was designed to sample and concentrate hydrophilic contaminants. It contains a sorbent phase sandwiched between two micro porous polyethersulfone membranes; chemicals diffuse from the water through the membrane and adsorb onto the sorbent phase. POCIS can provide Time-Weighted Average (TWA) concentration of contaminants in water if the sampling rates (Rs) are known. A calibration system for POCIS was developed and used to calculate the sampling rates of eight analytes belonging to pesticides, non-steroidal antiinflammatory drugs and perfluorinated compounds: atrazine, propazine, terbutylazine, diclofenac, ibuprofen, ketoprofen, perfluorooctanoic acid and perfluorooctane- sulfonate. Experiments with a linear velocity of 2.0, 5.1, 10.2 and 15.3 cm/s were carried out for 96 h using two different analyte concentrations. POCIS extracts were analyzed by liquid chromatography–tandem mass spectrometry (LC–MS/MS), using multiple reaction monitoring to maximize sensitivity. Results highlighted that the calculated sampling rates are rather constant at the considered concentrations and flow rates. The average sampling rates obtained with the calibration wer empoyed to assess the TWA concentration of the analytes in river and drinking waters. Results were in good agreement with the concentration levels usually detected in the considered real waters.


224

PE112 PRESSURISED HOTWATER EXTRACTION OF METAL ELEMENTS FROM TWO MORINGA PLANT SPECIES L. Chimuka*, P. Matshediso, E. Cukrowska, H. Tutu University of the Witwatersrand, 1 Jan Smut Avenue, Braamfontein, 2000 Johannesburg, South Africa

Moringa oleifera tree is now one of the most studied plant species because of its nutritional and medicinal health benefits. The tree is originally from India but is now widely grown throughout the world especially in tropical countries. Many countries in Africa are now forming Moringa associations to encourage its growth and use. In South Africa, besides Moringa association, the government through Department of Science and Technology is encouraging its growth and use especially for poverty alleviation. Many commercial and small scale farmers are thus growing Moringa. This study was aimed at looking at the elemental distribution in Moringa plant grown in South Africa using pressurized hotwater extraction followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis. Besides Moringa oleifera, Moringa ovalifolia native to Namibia was also extracted and results compared. Generally, the metals behaved differently at different temperature. In both Moringa sp, Na as compared to Ca, K and Mg increased with increasing extraction temperature. Among the macro nutrients extracted from the Moringa Oleifera, potassium was found to have highest concentrations than other metals at all extraction temperatures while in Moringa Ovalifolia Na and K competed for dominance. Trace elements like Fe and Al also tend to increase with increased extraction temperature in the two Moringa species.


225

PE113 MULTI-RESIDUE ANALYSIS OF PHARMACEUTICALS IN NGONG’ RIVER, KENYA, BY LIQUID CHROMATOGRAPHY - HIGH RESOLUTION MAGNETIC SECTOR MASS SPECTROMETRY K.O. K’oreje, L. Vergeynst, P. De Wispelaere, H. Van Langenhove, K. Demeestere Research Group Environmental Organic Chemistry and Technology (EnVOC), Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent, Belgium

The increasing global consumption of pharmaceuticals, their frequent trace detection in the environment and reported ecological effects have raised concern about these environmental emerging contaminants. Though a lot of research in this area is on-going in the developed world, there is limited data from developing regions, especially Africa. This study presents unique data by using a recently developed multi-residue analytical method based on solid-phase extraction (SPE) and liquid chromatography coupled to high resolution magnetic sector mass spectrometry (HRMS) to analyze Ngong’ River water (Kenya) towards the occurrence of 43 prioritized pharmaceuticals. Particular attention has been paid to the method validation for this kind of highly loaded (COD, TSS, TDS,...) river water. Based on well-thought decision criteria, taking into account the analyte stability both in solvent and on the SPE sorbent as well as the method’s process efficiency (optimum 60-140%) and precision, the compounds are categorized into four method quality labels, representing qualitative (class C), indicatively quantitative (class B1 and B2) and fully quantitative (class A) analysis. The study shows the occurrence of 20 pharmaceuticals, including scarcely investigated types like antiretroviral drugs, in the Ngong’ River with concentrations ranging from 3 ng/L to 15 μg/L. Nevirapine (antiretroviral), paracetamol (analgesic), sulfamethoxazole and trimethoprim (antibiotics) are the most frequently detected compounds.


226

PE114 FAST

AND

SENSITIVE

ALKYLIMIDAZOLIUM

SIMULTANEOUS

IONIC

LIQUID

SEPARATION

MICELLES

IN

OF

CATICHINS

BY

SWEEPING-MICELLAR

ELECTROKINETIC CHROMATOGRAPHY

Hassan Mabrook Albishri* and D. Abd El-Hady

*Chemistry Department, Faculty of Science, King Abdulaziz University, Saudi Arabia, Email: [email protected]

A rapid, sensitive and selective sweeping-micellar electrokinetic chromatography (sweeping-MEKC) method using 1-tetradecyl-3-methylimidazolium bromide (C14MImBr) as a sweeping carrier was firstly investigated for the simultaneous determination of catechins. The separation was performed by the micellar running buffer consisted of C14MImBr and phosphate buffer. The sweeping sample matrix was prepared in phosphate buffer free of IL micelles and injected hydrodynamically at 50 mbar for 250 s without compromise the separation efficiency. The practicality of the proposed method was validated by the quantitative determination of analytes in plasma based on the ICH guideline. The method was precise (RSD 0.5-1.5%, intraday precision), accurate (recovery 96-103%) and achieve adequate resolution between the catechins (resolution factor is more than 2.0). Limits of detections (LODs) of analytes at 200 nm were ranged from 0.09 to 5 ng mL-1. This could be due to the fascinating properties of C14MImBr including high conductivity and ability to form micelles in low concentrations.


227

PE 115 TOXICITY ASSESSMENT OF METOLACHLOR TOWARDS DIATOMS: COMBINING PHYSIOLOGICAL AND BEHAVIORAL ENDPOINTS

A. Gandon, N. Coquillé, G. Jan, N. Mazzella, S. Morin Irstea, UR EABX, F-33612 Cestas Cedex, France

The use of fertilizers in agriculture has a well-known effect on river, lake and coastal sea eutrophication. The effect of agricultural pesticides on aquatic ecosystems has been less investigated. Pesticides are transferred to the rivers via soil water runoff and spray drift. The toxicity of pesticides can affect non-target aquatic organisms and thus perturbate ecosystems. Herbicides may be toxic especially for aquatic photosynthetic organisms including algae. As primary producers diatoms are at the basis of the lotic trophic web. They have been extensively used as bioindicators of trophic and organic pollution. However, diatom standard indicators fail to properly detect toxic impact of molecules which do not target the photosystem II. The aim of the study is to evaluate the effect of an herbicide, the metolachlor (a cell division inhibitor) on a diatom species isolated from the field (Gomphonema gracile), exposed to three concentrations of metolachlor (1, 10, 100μg/L). Assessing metolachlor toxicity is metolachlor on diatoms were evaluated according to physiological and behavioral parameters. These parameters were analyzed immediately after exposure, and 1, 2, 3, 4 and 7 days post-exposure. Metolachlor didn’t affect much population dynamics, photosynthesis and ATP content. Though metolachlor didn’t bioaccumulate in the biota, the mobility parameters provided early responses (on day 3) for all concentrations. These finding demonstrate the importance of use of various parameters and the potential of behavioral descriptors in toxicity assessment.


228

PE 116 NANOSTRUCTURED ZnO/PDMS UV SENSORS

B. A. Albiss1*, M-Ali AL-Akhras2 and I. M. Obaidat3

1

Nanomaterials and Magnetism Lab, Jordan University of Science and Technology, Irbid, Jordan.

2

Bio-Medical Physics Lab, Physics Depart, Jordan University of Science & Technology, Irbid, Jordan.

3

Physics Department, United Arab Emirates University, Al-Ain, UAE

A highly sensitive, low-cost, high performance, flexible, reproducible UV sensor has been fabricated based on ZnO nanostructures embedded in polydimethylsiloxane (PDMS) elastomer. The ZnO nanostructures were synthesized via simple low temperature hydrothermal method. Several parameters were investigated during the fabrication process, including the heat-treatment, ZnO seeds density and concentration, pH and time of hydrothermal reaction solution and the thickness of the PDMS layer. The produced ZnO/PDMS nanocomposites were tested for their UV-sensing properties. Samples were characterized using scanning electron microscopy (SEM), x-ray diffraction (XRD), I-V characteristics and photoresponse measurements. All samples with different ZnO nanostructures responded to UV light but with different sensing characteristics. Such different responses could be attributed to the high surface-to-volume ratio of the nanostructure that correlated with the final ZnO micro/nanostructures formed at different synthesis parameters. For example, the UV-photoresponse mechanism of the ZnOnanorods/PDMS (ZnO-NP/PDMS) sensor with 15 wt% ZnO was analyzed. The sensor exhibited very high on/off ratios between photoresponse current and dark current. Under UV-irradiance of 10 mW/cm2 and bias voltage of 3 V, the photoresponse current reaches a maximum value of 0.2 mA and an on/off ratio of about 120 which is the highest among all samples used in this study. With PDMS filling the interspaces between nanorods, the ZnO-NR/PDMS sensor exhibited high optical transparency and excellent electronic conductivity and thus facilitated UV-light scattering to a deeper level in the nanorods networks. Therefore, upon the switching on of the UV light, more nanorods will receive UV photons, leading to the enhanced responsivity of the sensor. It is anticipated that the fabrication of ZnO-NR/PDMS UV sensor may have significant potential application in flexible optoelectronic devices.


229

PE118

THE ROLE OF OPERATIONAL PARAMETERS ON THE UPTAKE OF MERCURY BY DITHIOCARBAMATE FUNCTIONALIZED PARTICLES

D.S. Tavares, C.B. Lopes, A.L. Daniel-da-Silva, A.C. Duarte, T. Trindade, E. Pereira

University of Aveiro, Department of Chemistry, CESAM, CICECO, Institute of Nanotechnology, Campus de Santiago, 3810-193 Aveiro, Portugal

Sorbents based on silica and silica coated magnetite particles have been functionalized with dithiocarbamate (dtc) groups, aiming the uptake of mercury. Their uptake capacity was evaluated systematically for variable operational parameters including degree of functionalization, sorption time, sorbent dose and initial Hg concentration. It was possible to achieve uptake efficiencies > 99.5% in less than 24 h, regardless the sorbent dose, type of substrate and degree of functionalization, and all sorbents were able to decrease an initial Hg concentration of 50 µg/L to values circa 100 times lower than the guideline value for drinking water quality (1µg/L), with the additional advantage of magnetic separation by application of an external magnetic field, in the case of the silica coated magnetite. The high capacity of these materials toward Hg is attributed to their functionalization due to the strong complexation of the Hg and dtc groups. The modelling of the kinetic and the equilibrium results was well described by common kinetic and equilibrium equations. The authors thank Fundação para a Ciência e a Tecnologia (PTDC/CTM-NAN/120668/2010; PEstC/MAR/LA0017/2013; PEst-C/CTM/LA0011/2013), FSE and POPH for funding. The authors C.B. Lopes also thank their Post-DOC grants (SFRH/BD/45156/2008).


230

FOOD SAFETY

POSTERS !


"#$!

! PF1

Julius Arvay, Slovak University of Agriculture, Dept of Chemistry, Faculty of Biotechnology and Food Sciences, Nitra, Slovakia TRACE ELEMENTS AND TOTAL MERCURY CONCENTRATIONS IN VARIOUS TEAS (CAMELLIA SINENSIS) FROM ASIA

PF2

Aurélien Desmarchelier, Nestlé Research Center, Lausanne, Switzerland ON LINE EXTRACTION AND ANALYSIS OF OVER 70 ANTI-BIOTICS IN MILK POWDERS USING TURBULENT FLOW CHROMATOGRAPHY (TFC) COUPLED WITH LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY (LC-MS-MS)

PF3

Aurélien Desmarchelier, Nestlé Research Center, Lausanne, Switzerland EVALUATION OF THE EVIDENCE INVESTIGATOR PLATFORM FROM RANDOX FOR THE SCREENING OF DRUG RESIDUES IN MILK MATRICES

PF4

Mark Bücking, Fraunhofer Institute IME, Schmallenberg, Germany OCCURRENCE OF PFAS IN FOOD OF PLANT ORIGIN

PF5

Mark Bücking, Fraunhofer Institute IME, Schmallenberg, Germany DNA EXTRACTION FOR ANIMAL SPECIES DIFFERENTIATION IN PROCESSED FOOD USING T-RFLP

PF6

Rogerta Dalipi, Dipartimento di Ingegneria Meccanica e Industriale, Brescia, Italy TRACE ELEMENTS DETERMINATION IN ITALIAN WINES USING TOTAL REFLECTION X-RAY FLUORESCENCE

PF7

Elissavet Dotsika, Aghia Paraskevi, Attikis, Athens, Greece O-H-C ISOTOPES AS A TOOL FOR WINE AUTHENTICITY AND ORIGIN VALIDATION

PF8

Elissavet Dotsika, Aghia Paraskevi, Attikis, Athens, Greece C AND O ISOTOPES AS A TOOL FOR OLIVE OIL TRACEABILITY

PF9

Elissavet Dotsika, Aghia Paraskevi, Attikis, Athens, Greece ISOTOPES AS A TOOL FOR TRACEABILITY OF SHEEP MILK

PF10

Daniela Eisenstecken, Laimburg Research Centre for Agriculture and Forestry, Auer (Ora), Italy FATTY ACID PROFILING OF CHEESE FOR ORIGIN CONTROL – AN EXPLORATIVE APPROACH

PF11

Houssain El Aribi, AB Sciex, Brugg, Switzerland NON TARGET AND UNKNOWN SCREENING OF FOOD SAMPLES USING ACCURATE MASS LC-MS/MS SCREENING TECHNIQUES

PF12

Nadine Feichtmeier, University of Ulm, Institute of Analytical and Bioanalytical Chemistry, Germany APPLICATION OF SOLID SAMPLING HIGH-RESOLUTION-CONTINUUM SOURCE ATOMIC ABSORPTION SPECTROMETRY FOR THE DETECTION OF SILVER NANOPARTICLES IN FOOD SAMPLES


"#$!

! PF13

Nancy Frank, Nestlé Research Center, Lausanne, Switzerland QUANTIFICATION OF TRIS- (NONYLPHENYL)PHOSPHITE, AS A PRECURSOR OF THE ENDOCRINE DISRUPTORS 4-NONYLPHENOLS, IN FOOD PACKAGING MATERIALS

PF14

Eman M. Halawani, Taif University, Saudi Arabia GENETIC DIVERSITY AND ANTIMICROBIAL RESISTANT IN SALMONELLA ENTERICA CAUSING FOOD POISONING

PF15

Yves-Alexis Hammel, Nestlé Research Center, Lausanne, Switzerland CHEMICAL SCREENING STRATEGY TO VERIFY COMPOSITION AND COMPLIANCE OF PACKAGING MATERIALS

PF16

S.D. Lazi!, University of Novi Sad, Faculty of Agriculture, Novi Sad, Serbia LC/MS/MS DETERMINATION OF ACETAMIPRID RESIDUES IN SWEET CHERRIES

PF17

Rosa Antonia Lorenzo Feirreira, University of Santiago de Compostela, Dep. Analytical Chemistry, Spain EVALUATION OF CONTENT OF HIGH-INTENSITY SWEETENERS IN DIFFERENT CATEGORIES OF BEVERAGES AVAILABLE ON THE SPANISH MARKET

PF18

Hakimu Nsubuga, King Fahd University of Petroleum and Minerals, Dept of Chemistry, Dhahran, Saudi Arabia DETERMINATION OF TRACE-LEVEL EXPLOSIVE MARKER IN SEAFOOD USING MICROWAVE-ASSISTED ELECTROMEMBRANE EXTRACTION

PF19

Doris Poto"nik, Jo!ef Stefan Institute, Ljublijana, Slovenia DETERMINATION OF THE ADULTERATION OF MILK AND DAIRY PRODUCT BASED ON FATTY ACID COMPOSITION

PF20

Doris Poto"nik, Jo!ef Stefan Institute, Ljublijana, Slovenia DETECTION OF COW’S MILK IN SHEEP’S AND GOAT’S MILK AND CHEESES BY REAL-TIME PCR, 2-D ELECTROPHORESIS AND FATTY ACID COMPOSITION

PF21

Ailette Prieto Sobrino, University of the Basque Country/ Analytical Chemistry Department, Leioa, Spain SIMULTANEOUS EXTRACTION OF SEVERAL ENDOCRINE DISRUPTING COMPOUNDS IN VEGETABLES BY MEANS OF FOCUSED ULTRASONIC SOLIDLIQUID EXTRACTION AND DIFFERENT CLEAN-UP ESTRATEGIES

PF22

Diana N. Raba, Banat University of Agricultural Sciences and Veterinary Medicine, Timisoara, Romania ELECTROPHORETIC SDS-PAGE TECHNIQUE USED TO DISTINGUISH BETWEEN SOME WHEAT VARIETIES

PF23

Florina Radu, Banat University of Agricultural Sciences and Veterinary Medicine, Timisoara, Romania AFLATOXIN B1 CONTAMINATION OF ANIMAL FEEDS AND THE OCCURANCE OF AFLATOXIN M1 IN RAW COW MILK


"#%!

! PF24

Irena Staneczko-Baranowska, Silesian University of Technology, Faculty of Chemistry, Dept of Inorganic, Analytical Chemistry and Electrochemistry, Gliwice, Poland UHPLC-UV METHOD FOR THE DETERMINATION OF POLYPHENOLS IN DIETARY SUPPLEMENTS

PF25

Irena Staneczko-Baranowska, Silesian University of Technology, Faculty of Chemistry, THE INFLUENCE OF DIET RICH IN FLAVONOIDS ON THE DRUGS METABOLISM

PF26

Alena Vollmannova, Slovak University of Agriculture, Faculty of Biotechnology and Food Sciences, Nitra, Slovakia TOTAL POLYPHENOL CONTENT, TOTAL ANTIOXIDANT CAPACITY AND RISK ELEMENT CONTENT IN WILD AND CULTIVATED CRANBERRIES AND HIGHBUSH BLUEBERRIES

PF27

Renato Zanella, Federal University of Santa Maria, Chemistry Dep., Lab. of Pesticide Residues Analysis, &'()'!*'+,'!-!.&/!0+'1,2 SIMULTANEOUS MULTIRESIDUE METHOD FOR PESTICIDES AND VETERINARY DRUGS DETERMINATION IN BOVINE MILK BY LC-MS/MS

PF28

Pierre Zimmerli, Service de la consommation et des affaires vétérinaires, Geneva, Switzerland QUANTIFICATION OF HISTAMINE IN SELECTED CHEESES BY HILIC-MS/MS

PF29

M. Shoeb, Department of Chemistry, University of Dhaka, Dhaka, Bangladesh CHEMICAL CONTAMINANTS IN FOOD STUFF OF BANGLADESH

PF35

C. Durante, University of Modena and Reggio Emilia, Department of Chemical and Geological Science, Modena, Italy AN ANALYTICAL APPROACH TO THE DEVELOPMENT OF GEOGRAPHICAL TRACEABILITY MODEL OF OENOLOGICAL PRODUCTS

PF36

Özkan Özden, Dept of Seafood Processing and Quality Control, Faculty of Fisheries, Istanbul University, Laleli/ Istanbul, Turkey FATTY ACID CONTENT OF COMMERCIALLY IMPORTANT CULTURED FISH SPECIES FROM THE TURKEY

PF37

Nuray Erkan, Dept of Seafood Processing and Quality Control, Faculty of Fisheries, Istanbul University, Laleli/ Istanbul, Turkey THE SELENIUM CONTENT OF SMOKED, SALTED, DRIED, MARINATED AND COOKED FISHES

PF38

Suhendan Mol, Dept of Seafood Processing and Quality Control, Faculty of Fisheries, Istanbul University, Laleli/ Istanbul, Turkey DETERMINATION OF SELECTED TRACE METALS IN SHARKS (SQUALUS ACANTIAS) AND IN RAYS (RAJA CLAVATA)

PF39

M. Lommatzsch, TU Dresden, Chair of Food Science and Food Contact Materials, Dresden, Germany

ISSUES ON POSH MIGRATING INTO FOOD: COMPOSITION OF LOW MOLECULAR WEIGHT OLIGOMERS FROM POLYOLEFINS AND ANALYTICAL CHALLENGES 38th International symposium on environmental analytical chemistry !

"##!

! PF40

M. Lommatzsch, TU Dresden, Chair of Food Science and Food Contact Materials, Dresden, Germany

ONLINE COUPLED LC-LC(AG+)-GC-FID: ANALYSIS OF COMPLEX HYDROCARBON MIXTURES AS FOOD CONTAMINANTS PF42

Loïc Beyet, AB SCIEX. Les Ulis, France AUTOMATED DERIVATIZATION, SPE CLEANUP AND LC-MS/MS DETERMINATION OF GLYPHOSATE AND OTHER POLAR PESTICIDES

PF43

C. Jabot, Institute for Analytical Sciences, 5 rue de la Doua, Villeurbanne, France IDENTIFICATION OF PESTICIDE METABOLITES ON HONEYBEES

PF44

Andrea Beck, Nestlé Research Centre, Nestec Ltd, Lausanne, Switzerland EVALUATION OF THE EVIDENCE INVESTIGATOR PLATFORM FROM RANDOX FOR THE SCREENING OF DRUG RESIDUES IN MILK MATRICES

PF45

Marie-Claude Savoy-Perroud, Nestlé Research Centre, Nestec Ltd, Lausanne, Switzerland ON LINE EXTRACTION AND ANALYSIS OF OVER 70 ANTIBIOTICS IN MILK POWDERS USING TURBULENT FLOW CHROMATOGRAPHY (TFC) COUPLED WITH LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY (LC-MS-MS)


344!

PF1 TRACE ELEMENTS AND TOTAL MERCURY CONCENTRATIONS IN VARIOUS TEAS (CAMELLIA SINENSIS) FROM ASIA

J. Árvay, A. Vollmannová, T. Tóth, J. Musilová, M. Kopernická, !. Harangozo, J. Bystrická

Department of Chemistry, Faculty of Biotechnology and Food Sciences, Slovak University of Agriculture in Nitra, Trieda A. Hlinku 2, 949 76 Nitra, Slovak Republic.

Tea (Camellia sinensis, Linn.) is one of the most frequently consumed beverages in the world, dating back to more than 5000 years ago. Numerous studies have recorded the beneficial effect of the, e.g., antioxidant, anti-carcinoma, arteriosclerosis prevention and invigorating effects. In the present work, we have focused on the assessment of the level of contamination of commercially produced different kinds of tea with heavy metals (Hg, Cd, Pb, Zn, Cu, Ni, Co and Cr) of various areas in Central and Eastern Asia (China, Japan, Taiwan, Nepal, India). The samples of tea used for this study (n = 48) represent 5 characteristic groups of tea, which are sought by consumers. We performed analyses for the determination of the total mercury content and the content of other heavy metals by F-AAS respectively GF-AAS. The results of analyses were compared with the limit values of the risk metals that are defined by the legislative standard valid in the Slovak Republic and the EU. We evaluated the real impact on the level of the human body intoxication by regular consumption of beverages prepared from tea samples. We have calculated the tolerable weekly income of each of the heavy metals. Subsequently these values were compared with the values of TWI established by the European Food Safety Authority.

The Paper was supported by the Operational Program: Education, ITMS code: 26110230085


201

PF2 ON LINE EXTRACTION AND ANALYSIS OF OVER 70 ANTI-BIOTICS IN MILK POWDERS USING TURBULENT FLOW CHROMATOGRAPHY (TFC) COUPLED WITH LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY (LC-MS-MS)

Presenting author: Aurélien Desmarchelier M-Cl. Savoy-Perrouda, Y-A. Hammela and K. Kraehenbuehla Nestlé Research Center, Lausanne, Switzerland

Over 300 veterinary drugs are used in modern agriculture and residues are regulated for food raw materials of animal origin to ensure consumer’s safety. Recently the analytical approach for monitoring drug residues has rapidly evolved from single compound or family methods towards large multiresidue methods. A new TFC-LC-MS-MS method for the quantification of over 70 antibiotics in milk powders has been developed and validated. A new fully automated sample extraction technology (Turbulent Flow Chromatography (TFC)) was used which significantly decreases operator and turnaround time. Positive identification of antibiotics in matrix was conducted according to the confirmation criteria defined in EU Commission Decision 2002/657/EC while quantification was performed by one single point standard addition. The developed method was found fit for purpose for the quantification of over 70 antibiotics in the concentration range 0.5 to 1.5 Maximum Residue Limit (MRL) in reconstituted milk beverage and infant formulae. Other performance parameters like linearity [(r)2>0.98], recovery [70-120%], precision [(RSDr) and RSDiR) < 30%], and trueness [x-x%] were evaluated successfully. For some target analytes, the recoveries were 120-130 % or slightly above. It was shown that for these compounds the trueness was improved when using multipoint standard addition rather than single point.


202

PF3 EVALUATION OF THE EVIDENCE INVESTIGATOR PLATFORM FROM RANDOX FOR THE SCREENING OF DRUG RESIDUES IN MILK MATRICES

Presenting author: Aurélien Desmarchelier A. Beck a) & Cl. Mujahid a) a)

Nestlé Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland

The Evidence Investigator platform from Randox Food Diagnostics is a semi-automated bench top analyzer that uses biochip array technology and immunological detection similar to competitive ELISA and delivers semi-quantitative results using external calibration curve. The platform was evaluated for the screening of a large range of veterinary drugs in raw milk and milk derivatives. Five test arrays were selected for regulated antibiotics (Array ß-lactams, Array I sulfonamides, Array II tetracyclines, quinolones & others and Array IV aminoglycosides & macrolides), two for banned antibiotics (Array III Chloramphenicol milk only and Array III Chloramphenicol and nitrofurans) and one for nonantibiotic veterinary drugs (Anthelmintics array). In total 78 veterinary drug compounds were tested using six different arrays in this evaluation. Out of 78 target analytes, 67 were detectable at concentrations between 0.5 µg/kg and 10 µg/kg. The result for key compounds such as penicillin could also be confirmed in milk derivatives such as lactose and whey powders. Penicillin was detected at 1 µg/kg for all matrices. In our hands the Anthelmintics Array was not reproducible for milk matrices. Overall the results of the evaluation showed a broad coverage of all key antibiotics and several banned veterinary drugs for milk. A good sensitivity was obtained with minimal sample preparation for milk matrices (raw milk and milk fractions).


203

PF4 OCCURRENCE OF PFAS IN FOOD OF PLANT ORIGIN

M. Bücking, M. Kotthoff, H. Jürling and J. Müller

Fraunhofer-Institute for Molecular Biology and Applied Ecology IME, Auf dem Aberg 1, Schmallenberg, Germany

The investigation was performed within the framework of the EU FP7 project “Perfood”. The uptake of Perfluoroalkyl acids (PFAAs) from fortified soil into crops under field conditions was studied. The work complements a comparable study performed under controlled conditions (greenhouse hydroponic systems) at the University of Amsterdam. Corn, peas, radish and lettuce were planted on soils fortified to 4 PFAS levels (0.1 mg/kg, 1 mg/kg, 5 mg/kg and 10 mg/kg + unfortified soil). The tests were performed using soil lysimeters which allowed the collection of drainage water. After harvest the plant organs were analyzed for their contents of 11 perfluorocarboxylic acids (C4C14) und 2 perfluorosulfonic acids (PFBS and PFOS). In addition the PFAS were determined in the matrices soil, soil pore water and lysimeter drainage water. An overview is given over the performance of the study including site preparation, plant growing, analyses and results obtained.


204

PF5 DNA EXTRACTION FOR ANIMAL SPECIES DIFFERENTIATION IN PROCESSED FOOD USING T-RFLP

M. Bücking1, C. Diaz1, F. Cicotti2 and F. Carraturo2

1

Fraunhofer-Institute for Molecular Biology and Applied Ecology IME, Schmallenberg, Germany

2

University of Naples “Federico II” – Department of Biology, Hygiene Laboratories, Naples, Italy

The identification of animal species in meat and meat products is of great importance in the context of quality assurance for food and feed processing industries. Fraunhofer Institute has developed a T-RFLP method for animal species differentiation, in order to reach the target and overcoming the problem, for the processing industry, to examine raw products and highly elaborated food labeling.the processing of those matrices, whose animal species determination turned out to be critical due to DNA degradation levels, linked to industrial treatment steps (heating, freezing, etc.). The aim of this work was to evaluate a DNA extraction protocol to obtain high purity levels and extraction yields, from highly processed food and feed products. For this purpose, ready to eat meals containing meat in different percentages (from 3.4-87%), undergone through several degrees of processing, were purchased from the supermarket. The DNA from samples was extracted using a modified CTAB protocol: the employed method allowed DNA extraction yields in 300-4000 ng/µL range, with purity ratios (Abs 260/280) between 1.8-2.0. With the developed protocol, efficient DNA extraction and successful animal species identification with the T-RFLP method were achieved.


205

PF6 TRACE

ELEMENTS

DETERMINATION

IN

ITALIAN

WINES

USING

TOTAL

REFLECTION X-RAY FLUORESCENCE

R. Dalipi1, L. Borgese1*, A. Zacco1, K. Tsuji2, E. Bontempi1 and L.E. Depero1

1)

Department of Mechanical and Industrial Engineering, University of Brescia, Italy

2)

Graduate School of Engineering, Osaka City University, Japan

*Corresponding author: [email protected]

Total reflection X-ray fluorescence (TXRF) is a powerful technique for elemental chemical analysis. Simultaneous identification of major and trace elements in different matrices makes TXRF an emerging technology in the field of food analytics. Simple and fast screening of samples is possible as well as a reliable quantitative analysis, making TXRF suitable for the evaluation of food safety. Elemental analysis of wine is important for detection of essential elements but also to assess the presence of potentially toxic contaminants that may affect human health, such as As, Al, Cd, Cr, Cu, Pb and Ni. In this work TXRF was successfully used for elemental analysis of Italian wine samples. Quantitative analysis was performed by means of internal standard addition. To demonstrate the reliability of TXRF, direct TXRF analysis was performed in two different laboratories, in Italy and in Japan. Dehydration was also considered as a suitable conservation procedure. Traces of Mn, Ni, Zn and Pb were found in most of the samples, in concentrations lower than the levels established by The International Organization of Wine and Vine. Results show that TXRF is suitable to perform fast and simple direct analysis of wine sample and that dehydration is an effective way to store wine samples for further TXRF analysis.


206

PF7 O-H-C ISOTOPES AS A TOOL FOR WINE AUTHENTICITY AND ORIGIN VALIDATION Dotsika E.1, 2*, Chantzi P.2, Raco B.1, Karalis P.2 1

Institute of Geosciences and Earth Resources, Via G. Moruzzi 1, 56124 Pisa, Italy.

2

Stable Isotope Unit, Institute of Nanoscience and Nanotechnology, NCSR Demokritos, 15310 Agia

Paraskevi Attiki, Greece, [email protected] *

Corresponding author. Tel.: +30 210 6503305; Fax: +30 210 6519430 E-mail address:

[email protected]

The unequivocal uniqueness of Greek wines is resulted by the combination of the Greek terroir and the high quality of local wine varieties; therefore the authenticity control and origin assignment of Greek wine products have obtained remarkable importance. Stable isotopes have been applied for the reliable proof of wine authenticity and origin validation. Stable isotope analysis of 18O/16O, D/H and 13C/12C ratio in Greek wines and wine water was carried out in Stable Isotope Unit of Nanoscience & Nanotechnology Institute in N.C.S.R. Demokritos in order to be detected the geographical origin of the products. Specifically, the analyses of "13C in ethanol and wines water "18O reflect both the photosynthetic pathway and the climatic condi-tions of vine maturation. Resulted values of "18O were in a good agreement with those that referred to hot European counties with high precipitation potential. Greek wines presented "18O isotopic values range between -1.4‰ to 6‰ reflecting the different vintage years and conse-quently the different corresponding climatic factors (annual temperature, humidity). Generally the earlier the grape varieties mature the higher the "18O values of the wine water result. Moreover isotopic analysis of "18O and "2H was carried out not only in wine products but also in grape berries as the 18O contents of grape berries will be the tracer in final product. This based on the fact that 18O-2H relation of grape berries linked to the local water which characterize the wine growing region. Finally isotope values of "13C in ethanol for all vintage years of each wine type range between -27.9‰ to -23.1‰ confirming the origin of C3 plants which implies authentication of the wine product and not adulteration with industrial alcohol.


207

PF8 C AND O ISOTOPES AS A TOOL FOR OLIVE OIL TRACEABILITY Dotsika E.1, 2*, Leodiadis L.3, Poutoukis D.4, Karalis P2. 1

Institute of Geosciences and Earth Resources, Via G. Moruzzi 1, 56124 Pisa, Italy.

2

Stable Isotope Unit, Nanoscience and Nanotechnology, NCSR Demokritos, 15310 Agia Paraskevi

Attiki, Greece, [email protected] 3

Mass Spectrometry and Dioxin Analysis Laboratory, IRRP, NCSR Demokritos, 15310 Athens,

4

General Secretariat for Research and Technology, 10-14 Messogion, Athens, Greece

*

Corresponding author: [email protected]; Tel +302106503305; Fax+302106519430

Olive constitutes one of the earliest fruit trees that were cultivated by people, famous both for its oil and as edible fruit. The olive oil stars in Mediterranean diet as its components (oleic acid, linoleic acid etc) offer a protective effect with respect to health perspective; for this reason its demand presents an increase. Greece has a significant tradition in olive oil production so the identification of the Greek olive oil by variety and by origin is of crucial importance. The isotope ratio mass spectrometry (IRMS) has been introduced as a robust analytical method in the field of food authenticity and origin control. Stable isotopes of carbon and oxygen widely applied and provide valuable information on food authentication perspective. Stable carbon isotope (13C/12C) and stable oxygen isotope (18O/16O) of thirty nine olive oil samples from Greece (31 samples from Peloponnese, 2 from Crete, 3 from Andros, 1 from Mytilene, 1 from Boeotia and 1 Fthiotida) were performed in Stable Isotope Unit of Nanoscience & Nanotech-nology Institute in N.C.S.R. Demokritos in order to be determined the purity and origin of Greek olive oils. Data ranges from -27.1‰ to -28.9‰ for "13C and from 22‰ to 24.1‰ for "18O. Based on the results it is concluded that isotopic values are strongly affected by the climate regime. This is well highlighted at the sample from Fthiotida which differs from all samples. It is seemed that on the direction from North to east the values became more positive as the value of "13C for Fthiotida (and Mytilene) is -28.9‰ (-28.4‰ for Mytilene) while for Hrakleio in Crete is -27.1‰. These "13C values correspond well to those characteristic of C3 plants confirming the authentication of Greek olive oil product. Moreover the mountainous area of Fthiotida participates to the isotopic values forming. Lower temperature and higher moisture at high altitudes are the predominant control factors of "13C variation in plants. Moreover "18O values differ about 2" from those values that correspond to neighbor countries. This fact is attributed to the vicinity of the study areas with sea (less than 60km).


208

PF9 ISOTOPES AS A TOOL FOR THE TRACEABILITY OF SHEEP MILK Dotsika E.1, 2, Raco B.1, Bulleri E.3, Mele M.3, Battaglini R.4, Poutoukis D.5 Chantzi P.2 1 Institute of Geosciences and Earth Resources, Via G. Moruzzi 1, 56124 Pisa, Italy. 2 Stable Isotope Unit, Institute of Materials Science, NCSR Demokritos, 15310 Agia Paraskevi Attiki, Greece, [email protected] and Institute of Geosciences and Earth Resources, Via G. Moruzzi 1, 56124 Pisa, Italy 3 Dipto di Scienze Agrarie, Alimentari e Agro-ambientali, via del Borghetto 80, 56124 Pisa, Italy 4 TerreLogiche, via Verdi 3, 57021Venturina Terme (LI), Italy. 5 General Secretariat for Research and Technology, 10-14 Messogion, Athens, Greece The ability to authenticate the origin of a product has become increasingly important and enhances local and/or typical production. Among the various analytical techniques, with direct and indirect tracing indicators that used to identify the geographical origin of individual products and systems of food production, isotopic traceability represents one of the most promising methods. For this reason, considering the presence of Italian excellence in the production of cheese in Tuscany, was decided to be tested, for Pecorino Toscano DOP, within the territory of reference of the DOP, the ability to determine the geographical origin of sheep milk depending on its the isotopic composition of oxygen-18 ("18O) and deuterium ("2H) as well as the isotopic composition of livestock watering water. For this study two different geographical areas were selected, both important in the tradition of cheese: Tuscany and Sardinia. So, analyzes of "18O and "2H on water watering and milk product were performed for the samples that were collected from 4 farms located in Manciano (GR), members of Manciano Cheese Factory in Stable Isotope Unit of Institute of Nanoscience & Nanotechnology in N.C.S.R. Demokritos. It was further determined the isotopic content of carbon-13 ("13C) and nitrogen-15 ("15N) of the feed supplied to livestock in order to assess the possibility of using these parameters to characterize the geographical origin. The same analyzes were performed on samples from 4 farms located in northern Sardinia (Porto Torres) thanks to the collaboration of Prof. Anna Nudda the Dept. of Agriculture of the University of Sassari. For water watering, the values of "18O‰ and "2H‰ in Tuscany range from -8.3 to -6.3‰ and from -53 to -41‰ respectively while for Sardinia range from -6.9 to 5.8‰ and from -38 to -34‰. For milk product, oxygen-18 isotopes and deuterium range from -1.9 to 1.8‰ and from -25 to -8‰ respectively while for Sardinia range from 1.0 to 2.0‰ and from -25 to -20‰. The correlation between stable isotopes of milk and watering water showed different trends of isotope enrichment for Sardinia and Tuscany samples. Albeit with due caution, the two regression lines allowed us to distinguish the Tuscan milk from Sardinian milk, confirming the two different origin zones. The isotopic values of 13C and 15N for Tuscany feed samples range from -29‰ to -25.1‰ and from 2.0‰ to 4.2‰ respectively while for Sardinia range from -28.1‰ to -23.6‰ and from 3.2‰ to 6.2‰. The feed samples presented a typical composition of "13C for C3 plants; however, samples from Sardinia were characterized by an average isotopic composition more depleted in 13C compared to those of Manciano while the exact inverse trend presented regarding the content of 15N/14N. This has been mainly attributed to the different rainfall regime of the study areas. Results showed that the isotopic ratios of "2H and "18O in water as well as of "15N and "13C in feed supplied to livestock, correlated to the origin area. In fact, the climatic and geographical disparity of study areas, Tuscany and Sardinia, have an impact on isotopic composition of the sheep livestock watering water and on the isotopic composition of local agricultural production.


209

PF10 FATTY ACID PROFILING OF CHEESE FOR ORIGIN CONTROL – AN EXPLORATIVE APPROACH

D. Eisenstecken1, P. Robatscher1, C. W. Huck2, L. Kerschbaumer3, and M. Oberhuber1

1

Laimburg Research Centre for Agriculture and Forestry, Pfatten (Vadena) 6, 39040 Auer (Ora), Italy

2

Leopold-Franzens University, Institute of Analytical Chemistry and Radiochemistry

Innrain 80-82, 6020 Innsbruck, Austria 3

Sennereiverband Südtirol, Galvanistraße 38, 39100 Bozen (Bolzano), Italy

The complex fatty acid (FA) profiles of cheese provide important information on diet composition and ruminal fermentation pattern and thus can be used to address authenticity issues. In this study, the FA profiles (approx. 40 acids) in cheese samples and their corresponding milk samples from various alpine origins were determined using high-resolution gas chromatography and subsequent multivariate data analysis. First results of principal component analysis (PCA) show a good separation between cheese produced from cow’s milk of mountain pastures (> 1900 m.a.s.l.) and cheese from bulk milk from the valleys. The discrimination is mainly due to higher concentrations of unsaturated fatty acids (UFA) and stearic acid (C18:0) as well as lower amounts of saturated fatty acids (SFA) in cheese from alpine pastures. Explorative data analysis on the same cheese type produced in two different dairies located approximately 150 km apart shows a possible distinction regarding the origin. The most influencing FAs for the multivariate approach are UFAs with concentrations below 1.0 mg/100 mg fat. Further experiments addressing the verification of these preliminary results will indicate the potential of FA fingerprinting for origin control.


210

PF11 NON-TARGET AND UNKNOWN SCREENING OF FOOD SAMPLES USING ACCURATE MASS LC-MS/MS SCREENING TECHNIQUES

Houssain El Aribi3 and André Schreiber1, David Cox1, Jianru Stahl-Zeng2, Julia Jasak2 1

AB SCIEX; 71 Four Valley Drive, Concord, ON, Canada;

2

AB SCIEX; Darmstadt, Germany

3

AB SCIEX; Steinbruchstrasse 11, 5200, Brugg, Switzerland; [email protected]

Liquid Chromatography coupled to tandem Mass Spectrometry (LC-MS/MS) is a powerful analytical tool for the analysis of polar, semi-volatile, and thermally labile compounds of a wide molecular weight range, such as pesticides, veterinary drugs, mycotoxins and other food residues and contaminants. Mass analyzers based on triple quadrupole technology operated in Multiple Reaction Monitoring (MRM) mode deliver highly selective and sensitive quantitative results and are therefore well established for multi-target screening and quantitation of food contaminants. However, the use of triple quadrupole based mass analyzers limits the number of compound to quantify and identify. In addition there is an increasing demand for retrospective non-target (unknown) data analysis to identify unexpected food residues and contaminants. High resolution and accurate mass instruments are capable of performing targeted and non-targeted screening in a single LC-MS/MS run. Here, a generic QuEChERS procedure was used to extract residues and contaminants from fruit and vegetable samples. Extracts were subsequently analyzed by LC-MS/MS using the AB SCIEX TripleTOF® system operated in high resolution accurate mass MS and MS/MS mode. Non-Target compounds were identified based on non-target peak finding and sample control comparison to separate chemicals of interest from matrix components. Accurate mass MS and MS/MS information was used to empirically calculate molecular formulae. Found molecular formulae war searched against ChemSpider to find matching structures. Structures were automatically compared against the MS/MS spectrum and theoretically fragmented to tentatively identify the detected compound. Data processing was performed in MasterView™ software was allows quick processing and intuitive data review. Keywords: pesticides, accurate mass, time-of-flight, TOF, LC-MS/MS, unknown, identification


211

PF12 APPLICATION OF SOLID SAMPLING HIGH-RESOLUTION-CONTINUUM SOURCE ATOMIC ABSORPTION

SPECTROMETRY FOR THE

DETECTION

OF

SILVER

NANOPARTICLES IN FOOD SAMPLES

N. Feichtmeier and K. Leopold

University of Ulm, Institute of Analytical and Bioanalytical ChemistryAlbert-Einstein-Allee 11, 89081 Ulm, Germany

Silver nanoparticles (AgNPs) find use in many fields, such as in optical sensors, textile engineering, electronics, optics, biosensing, and in medical applications as bactericidal agent. In the last years, AgNPs-containing nanomaterials are increasingly implemented in food industry and research, e.g. for impregnation of fridges, cutting boards and food storage boxes in order to prevent bacterial growth. In this regard several workers have suggested immission of AgNPs into the food chain. Regarding unforeseen effects of silver nanoparticles their detection and quantification in food is of great importance. In the present study different food samples, such as parsley, apple, noddles that were either spiked with AgNPs or came into contact with AgNP-impregnated surfaces were investigated for the presence of AgNPs. For this purpose a novel direct solid sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) was applied. This method was recently developed in the Leopold research group and omits any time-consuming sample pretreatment steps. Here, AgNPs can be identified in solids by a new interpretation method of the absorbance signal providing clear distinction from ionic silver. The results obtained from investigation of several food samples demonstrate the feasibility of this approach.


212

PF13 QUANTIFICATION OF TRIS(NONYLPHENYL)PHOSPHITE, AS A PRECURSOR OF THE ENDOCRINE DISRUPTORS 4-NONYLPHENOLS, IN FOOD PACKAGING MATERIALS

N. Frank, P. Mottier, A. Tarrès, M. Dubois, T. Bessaire and T. Delatour Nestlé Research Centre, Nestec Ltd., Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland

Tris(nonylphenyl)phosphite (TNPP), an antioxidant used in polyethylene (PE) resins for food applications, is problematic since it is a source of the endocrine-disrupting chemicals 4-nonylphenols (4-NP) upon migration into packaged foods. This poster describes an analytical procedure to verify “TNPP-free” statement issued by resin producers and additive suppliers in multilayer laminates used for bag-in-box packaging. TNPP is extracted from laminates and analysed by LC-MS/MS. A subsequent acidic hydrolysis of such packaging extract allows the release of 4-NP from potentially extracted TNPP. 4-NP is analysed by LC-MS/MS as well. This two-step analytical procedure ensures not only TNPP quantification in laminates, but allows flagging possible other sources of 4-NP in such packaging materials, typically as non-intentionally added substances (NIAS). Though “TNPP free” statements had been obtained from suppliers, TNPP at levels up to 130 µg/dm2 was occasionally detected during quality control operations, evidencing some lack of traceability at the supplier level. Low TNPP contamination (up to 10 µg/dm2) was evidenced in some TNPP-free laminates as well and later on explained as cross-contamination of lamination equipment at the converter level when TNPPcontaining laminates are processed on the same machine beforehand.


213

PF14 GENETIC

DIVERSITY

AND

ANTIMICROBIAL

RESISTANT

IN

SALMONELLA

ENTERICA CAUSING FOOD POISONING

E. Halawani and M. Shohyeb [email protected] Department of Biology, Faculty of Science, Taif University, Saudi Arabia

Food-borne Salmonella infections are responsible for 1.3 million illnesses annually worldwide, resulting in 16,000 hospitalization and 600 deaths. The two predominant agents associated with foodborn nontyphoidal salmonellosis were S.enterica serotype Enteritidis and S.enterica serotype Typhimurium.We report the gentic diversity and antimicrobial resistance in clinical isolates of salmonella entrica Serotype Typhimurium(23) and serotype Enteritidis(18) using plasmid profile and antibiogram analysis.

Isolates of both serotypes harbored a sero-specific high molecular weight

plasmid; 90 kb in Salmonella serotype Typhimurium and 60 or 65 kb in serotype Enteritidis. In addition 82.6% and33.3% of the isolate in Salmonella serotype Typhimurium and serotype Enteritidis, harbored one or more low molecular weight plasmids. It was possible to recognize 7 and 5 plasmid profiles in both serotypes Typhimurium and Enteritidis respectively. Dicecoefficient analysis of plasmids revealed 4 clusters in serotype Typhimurium with 7 sub-clones and 3 clusters with 6 subclones in serotype Enteritidis. Cluster A in serotype Typhimurium was more prominent (69.6% of isolates) and cluster E was more prominent in serotype Enteritidis (61.1% of isolates)in Saudi Arabia . Multi-drug resistance was prevalent in the majority of isolates of Salmonella Typhimurium and more than 70% of these isolates were resistant to 6-8 antibiotics with 10 antimicrobial resistant phenotypes, while Salmonella Enteritidis isolates were mostly resistant to streptomycin, neomycin and Sulfamethoxazole and 3 resistant patterns were detected. When both plasmid profiles and antibiograms were combined the sub-clones were further divided into several new sub-clones up to 21

Data

obtained suggest that the misuse of antibiotics resulted in the development and the dissemination of new sub-clones of both serotypes outbreaks in the community. 38th International symposium on environmental analytical chemistry

214

PF15 CHEMICAL SCREENING STRATEGY TO VERIFY COMPOSITION AND COMPLIANCE OF PACKAGING MATERIALS

Yves-Alexis Hammel, Amaury Patin, Lionel Spack, Jésus Varela, Julien Veyrand, Sander Koster, Hervé Simian Nestlé Research Center, Lausanne, Switzerland The main criteria for the selection of a food contact packaging are that it should protect adequately the food during its shelf life and to conveniently deliver the product to the consumers. However, the food contact packaging should be compliant with applicable legislation, safe regarding the interaction with food and keep the quality of the food. As final user, Nestlé should verify the final compliance of the packaging materials and consequently organize monitoring and /or surveillance of the incoming packaging materials. The approach presented starts with 1) an extraction of the food contact materials (FCM) to extract as much substances present in the packaging materials followed if needed with 2) a migration experiment using a worst case simulant for a conservative evaluation. Goal of the extraction experiment (1) is to obtain a rough estimate of the chemical composition of a FCM, including substances that will not even migrate from the FCM into food. Both intentionally added substances (IAS) and non-intentionally added substances (NIAS) may be detected and, for the latter, classified as already known NIAS, newly identified NIAS or not identified NIAS. These extraction experiments are used to investigate for new FCM whether the overall composition of the FCM is in compliance with legislation and Nestlé requirements. Migration experiments into simulants (2) may be performed in addition to the extraction experiments to determine exposure to compounds found in the extraction step. The analytical screening procedures apply both for extraction or migration of the FCM and consist of a headspace GC-MS analysis of volatile molecules present in the FCM, a GC-MS/FID analysis of semivolatile molecules and an LC-HRMS (high resolution) analysis of non-volatile molecules. GC-MS is used for identification, GC-FID for semi-quantification. The LC-HRMS analysis makes use of a UPLC Q-Exactive operated in positive/negative electrospray ionization mode. This poster describes an extensive chemical screening procedure to cover as much as possible all IAS and NIAS that may be present in the FCM with a wide variety of physical/chemical properties.


215

PF16

LC/MS/MS DETERMINATION OF ACETAMIPRID RESIDUES IN SWEET CHERRIES

S.D. Lazi#1, P.T. Jovanov2, D.B. $unjka1, V.J. Guzsvany3

1

University of Novi Sad, Faculty of Agriculture, Trg Dositeja Obradovi#a 8, 21000 Novi Sad, Serbia

2

University of Novi Sad, Institute of Food Technology, Bulevar Cara Lazara 1, 21000 Novi Sad, Serbia

3

University of Novi Sad, Faculty of Science

In this study we have developed an analytical method for the determination of insecticide acetamiprid residues in sweet cherry samples. The QuEChERS method of extraction coupled with LC/MS/MS were carried out. Validation of the method is performed in accordance with SANCO/12495/2011 criteria. Obtained recoveries at six concentration levels (0.1-2.25 mg/kg) were between 86-98%. Precision expressed as relative standard deviation were 0.01% for the intraday precision. Acetamiprid showed linear calibration curve for concentrations from 0.05 to 2.5 µg/ml with R2 of 0.999%. Limit of quantification were established at 1.5 µg/kg. Matrix effect calculated as slope ratio of MMC and SC was 93.6%. The validated method was used in survey, carried out on samples collected in the orchards after applications of acetamiprid commercial formulation (200 g a.i./kg) in the rate of 0.025%. The samples are collected immediately after the application and every second day, during 14 days. In this observing period, the concentration of acetamiprid is decreased from 0.31 mg/kg to 0.09 mg/kg and after the PHI was below MRLs in Serbia and in EU (1.5 mg/kg). ACKNOWLEDGEMENT. This

research is a part of projects TR31038 and 114-451-4418/2013-03.


216

PF17 EVALUATION OF CONTENT OF HIGH-INTENSITY SWEETENERS IN DIFFERENT CATEGORIES OF BEVERAGES AVAILABLE ON THE SPANISH MARKET

R.A. Lorenzo1*, P. Fernández2, M. Regenjo2, M.T. Pena1, P. González1, A.M. Carro1 1

Dpto. Química Analítica, Nutrición y Bromatología. Facultad de Química, Universidad de Santiago de

Compostela, 15782 Santiago de Compostela, Spain 2

Dpto. Anatomía Patológica y Ciencias Forenses. Facultad de Medicina, Universidad de Santiago de

Compostela, 15782 Santiago de Compostela, Spain *Email address: [email protected]

The objective of this study was to develop an accurate and sensitive liquid chromatography method for a better control of the content of artificial sweeteners in industrial beverages. The analysis of 66 samples of different marks of beverage was performed by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). Monitoring was done on seven sweeteners: aspartame, neohesperidine dihydrochalcone, neotame, potassium acesulfame, saccharin, sodium cyclamate and sucralose in beverages marketed as "sugar-free" or "diet". Minimal sample preparation procedure consisting on a simple dilution and filtration is required. The method showed excellent linearity (R20.98], recovery [70- 120%], precision [(RSDr) and RSDiR) < 30%], and trueness [xx%] were evaluated successfully. For some target analytes, the recoveries were 120-130 % or slightly above. It was shown that for these compounds the trueness was improved when using multipoint standard addition rather than single point.


240

! ! !

! ! ! ! SEE YOU AT ISEAC39 and 2nd CONFERENCE of FOOD SAFETY 2016 in HAMBURG, Germany !

38th International symposium on environmental analytical chemistry ! !

"#$!