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Applications in High Resolution Mass Spectrometry: Food Safety and Pesticide Residue Analysis 1st Edition
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Library of Congress Cataloging‑in‑Publication Data
Names: Heinzen, Horacio, 1957- | Nollet, Leo M. L., 1948- | Rodríguez Fernández-Alba, Amadeo.
Title: Multiresidue methods for the analysis of pesticide residues in food / [edited by] Horacio Heinzen, Leo M.L. Nollet, Amadeo R. Fernandez-Alba. Description: Boca Raton : CRC Press, 2017. | Series: Food analysis & properties | Includes bibliographical references and index.
Identifiers: LCCN 2016059196 | ISBN 9781482235098 (hardback : alk. paper)
LC record available at https://lccn.loc.gov/2016059196
Visit the Taylor & Francis Web site at http://www.taylorandfrancis.com
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Foreword
Editors
Contributors xi
Section i ReGULAtoRY iSSUeS
Chapter 1 European Union Monitoring Programs 3
Paula Medina-Pastor
Chapter 2 Monitoring Programs in the United States 27
Chris Sack
Section ii SAMPLe PRePARAtion
Chapter 3 Most Common Sample Preparation Methods for Pesticide Residue Analysis: Ethyl Acetate Method, Mini-Luke, and Matrix Solid Phase Dispersion 53
Lucia Pareja and Ana Lozano
Chapter 4 Sample Preparation Methods for the Determination of Organic Micropollutants 99
Carlos Goncalves, Maria Augusta D. Sousa, Vasilios G. Samaras, and Leo M.L. Nollet
Chapter 5 QuEChERS and Other MRM Sample Preparation Methods: SPE, SPME, DLLME, SBSE, ASE, MAE, SFE 131
Silvina Niell, Natalia Besil, Marcos Colazzo, María Verónica Cesio, and Horacio Heinzen
Section iii AnALYSiS
Chapter 6 Gas Chromatography–Mass Spectrometry: Basic Concepts and Instrumentation 171
Basil K. Munjanja
Chapter 7 Liquid Chromatography Mass Spectrometry (LC-MS)
Basil K. Munjanja
Chapter 8 Gas Chromatographic Analysis of Pesticide Residues 235
Andrés Pérez-Parada
Chapter 9 Applications of LC-MS/MS in Pesticide Residue Analysis: An Overview 293
Dasharath Oulkar, Arnab Goon, and Kaushik Banerjee
Chapter 10 Time-of-Flight and Orbitrap Mass Spectrometry for Target and Nontarget Analysis of Pesticide Residues in Food 339
María del Mar Gómez-Ramos, Ana Lozano, Łukasz Rajski, and Amadeo R. Fernández-Alba
Chapter 11 Databases for Pesticide Residue Analysis 381
Juan F. García-Reyes, Patricia Pérez-Ortega, Bienvenida Gilbert-López, and Antonio Molina-Díaz
Chapter 12 QA/QC for Pesticide Residue Analysis
Stanisław Walorczyk
Foreword
In the last decades, public concern on pesticide residue content in foods has been rising steadily. The global development of food trade implies that aliments from everywhere in the world can reach the consumer’s table. Therefore, the identification of agricultural practices that employ different pesticide combinations and application rates to protect produce must be characterized, as these practices leave residues that could be noxious to human health. However, the possible number of pesticides (and its metabolites of toxicological relevance) to be found in a specific commodity is almost 1500, and the time needed to analyze them one by one makes this analytical strategy a nonrealistic task. Despite the problematic context, regulatory agencies all over the world have been trying to give an answer to this particularly important issue in order to ensure food safety from farm to fork.
To overcome this problem, the concept of multiresidue methods (MRMs) for the analysis of pesticide traces has been developed. By the end of the last century, MRM of pesticide residues entailed complex strategies combining time-consuming multisample preparation steps followed by gas chromatographic separations with specific and selective detection of the residues, where the positives in a sample had to be confirmed through laborious protocols. Liquid chromatography was scarcely employed, and as a consequence, residues of many nonvolatile and polar pesticides could not be analyzed properly.
The new century brought a radical change in concept on how to face the development of MRM of pesticide residues. The advent of new and highly sensitive instrumentation, based in hyphenated chromatographic systems to coupled mass analyzers (MS/ MS or MSn), permitted simultaneously the identification and the determination of up to hundreds of pesticide residues in a single chromatographic run. This approach boosted the broadening of the scope of the analysis of pesticide residues in a myriad of food and environmental matrices. The high efficiency of the instrumentation forced the fitting for purpose of the sample preparation protocols: Exhaustive cleanup of the sample were no longer needed and straightforward, miniaturized, and even automated sample preparation procedures are continuously being developed for specific and problematic matrices.
Lower detection and quantification limits allowed a stricter control of food contaminants, and the limit permitted for not allowed pesticides was brought to levels as low as 10 μ g/kg by the regulatory agencies, for example, the European Union, United States, Japan, and Russia challenging food exports from third countries and international regulations like the Codex Alimentarius.
After 10 years of systematic development of pesticide residue analysis in foods based on trace determination through different combinations of tandem mass spectrometers coupled to high-resolution chromatography methods, an in-depth discussion of the advances and future horizons in the field is needed. The book Multiresidue Methods for Pesticide Trace Analysis in Foods aims to update, cover, and revise critically the
analytical procedures developed in the literature, as well as those currently employed in the most advanced laboratories that perform routinely pesticide residue analysis. This specialized view pretends also to give the insights to starters willing to be involved in this discipline. In addition to these points, the regulations, guidelines, and recommendations from the most important regulatory agencies of the world on the topic will be commented and contrasted.
The editors of this book like to cordially thank all authors of the different chapters. They achieved excellent works. The editors appreciate all the work and time. As it is known, researchers all over the world have many duties but spare time to write book chapters.
The editors also like to thank all people at the publisher’s office, invisible, not named. However, their work is invaluable.
Great works are performed not by strength but by perseverance.
Samuel Johnson
Horacio Heinzen Leo M.L. Nollet Amadeo R. Fernández-Alba
Editors
Horacio Heinzen is a chemist of pharmacognosy (UdelaR, 1983) and earned his degree of Doctor of Göttingen University, Germany, in 1993. He is professor of pharmacognosy and natural products chemistry faculty, UdelaR, since 1998.
His main lines of research are the characterization of new bioactive compounds, the validation of the action of native medicinal plants, and the development of a new herbal. In the analytical area, he turned to the area of analysis of pesticide residues and organic contaminants. In particular, his works focus on the development of new analytical methodologies on the preparation of samples for the analysis of trace organic compounds in complex matrices, both food and pharmaceutical raw materials.
He is coauthor of more than 70 original papers in scientific magazines. He wrote many book chapters and he was a speaker at numerous conferences, national, regional, and international.
He was president of the Latin American Society of Phytochemistry (2005–2008) and he is a member of the International Union of Pure and Applied Chemistry and the Scientific Committee of the Latin American Pesticide Residue Workshop (LAPRW) Subcommittee for Crop Protection.
Leo M.L. Nollet received his MS (1973) and PhD (1978) in biology from the Katholieke Universiteit Leuven, Belgium. He is editor and associate editor of numerous books. He edited for M. Dekker, New York—now CRC Press of Taylor & Francis—the first, second, and third editions of the books entitled Food Analysis by HPLC and Handbook of Food Analysis. The last edition is a two-volume book. He also edited the Handbook of Water Analysis (first, second, and third editions) and Chromatographic Analysis of the Environment, Third Edition (CRC Press).
With F. Toldrá, he coedited two books published in 2006 and 2007: Advanced Technologies for Meat Processing (CRC Press) and Advances in Food Diagnostics (Blackwell Publishing—now Wiley). With M. Poschl, he coedited the book Radionuclide Concentrations in Foods and the Environment, also published in 2006 (CRC Press). Dr. Nollet has also coedited with Y. H. Hui and other colleagues several books: Handbook of Food Product Manufacturing (Wiley, 2007), Handbook of Food Science, Technology and Engineering (CRC Press, 2005), Food Biochemistry and Food Processing (first and second editions; Blackwell Publishing—now Wiley—2006 and 2012), and the Handbook of Fruits and Vegetable Flavors (Wiley, 2010). In addition, he edited the Handbook of Meat, Poultry and Seafood Quality, first and second editions (Blackwell Publishing— now Wiley—2007 and 2012).
From 2008 to 2011, he published with F. Toldrá five volumes on animal-productrelated books, namely, the Handbook of Muscle Foods Analysis, the Handbook of Processed Meats and Poultry Analysis, the Handbook of Seafood and Seafood Products
Analysis, the Handbook of Dairy Foods Analysis, and the Handbook of Analysis of Edible Animal By-Products. Also in 2011, with F. Toldrá, he coedited for CRC Press two volumes: Safety Analysis of Foods of Animal Origin and Sensory Analysis of Foods of Animal Origin. In 2012, they both published the Handbook of Analysis of Active Compounds in Functional Foods.
In a coedition with Hamir Rathore, the book Handbook of Pesticides: Methods of Pesticides Residues Analysis was marketed in 2009; Pesticides: Evaluation of Environmental Pollution, in 2012; and the Biopesticides Handbook, in 2015.
Other finished book projects include Food Allergens: Analysis, Instrumentation, and Methods (with A. van Hengel; CRC Press, 2011) and Analysis of Endocrine Compounds in Food (Wiley-Blackwell, 2011). Dr. Nollet’s recent projects include Proteomics in Foods with F. Toldrá (Springer, 2013) and Transformation Products of Emerging Contaminants in the Environment: Analysis, Processes, Occurrence, Effects and Risks with D. Lambropoulou (Wiley, 2014). In this series, CRC Food Analysis & Properties, he edited with C. Ruiz-Capillas Flow Injection Analysis of Food Additives (CRC Press, 2015) and Marine Microorganisms: Extraction and Analysis of Bioactive Compounds (CRC Press, 2016).
Amadeo R. Fernández-Alba is master in chemistry (University Complutense of Madrid) and professor in the area of analytical chemistry at the University of Almería. He is director/founder of the Group of investigation AGR 159 “Pesticide residues” of the Junta de Andalucía.
He is the author of more than 120 articles on analysis of contaminants in food and environment. He is editor of three books on control of residues of pesticides, both legislative and technical, and of control of quality. The majority of these works are related with the application of mass spectrometry. He is/was a speaker at numerous conferences and is a participant in more than 50 European and National (Spanish) projects mainly related with the evaluation of contaminants in food and environment. He is co-head of the Community Reference Laboratory for Pesticide Residues in Fruits and Vegetables and member of the European Committee European of Normalisation CEN WG4. He is counselor of the Andalusian service of health of the Junta of Andalusia for the control of food quality.
Kaushik Banerjee
National Referral Laboratory
Contributors
ICAR-National Research Centre for Grapes
Pune, India
Natalia Besil
Grupo de Análisis de Contaminantes
Traza (GACT)
Departamento de Química del Litoral
Centro Universitario Regional (CENUR)
Litoral Norte
Universidad de la República (UdelaR) Montevideo, Uruguay
María Verónica Cesio
Grupo de Análisis de Contaminantes
Traza (GACT) Pharmacognosy
Facultad de Quimica and
Grupo de Análisis de Contaminantes
Traza (GACT) Holistic Pole on the impact of Agrochemicals
Universidad de la República (UdelaR) Montevideo, Uruguay
Marcos Colazzo
Grupo de Análisis de Contaminantes
Traza (GACT)
Departamento de Química del Litoral
Centro Universitario Regional (CENUR)
Litoral Norte
Universidad de la República (UdelaR)
Montevideo, Uruguay
Amadeo R. Fernández-Alba
European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables (EURL-F&V)
Agrifood Campus of International Excellence (ceiA3)
Department of Physics and Chemistry
University of Almeria
Almería, Spain
Juan F. García-Reyes
Analytical Chemistry Research Group
Department of Physical and Analytical Chemistry
University of Jaén
Jaén, Spain
Bienvenida Gilbert-López
Analytical Chemistry Research Group
Department of Physical and Analytical Chemistry
University of Jaén
Jaén, Spain
María del Mar Gómez-Ramos
European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables (EURL-F&V)
Agrifood Campus of International Excellence (ceiA3)
Department of Physics and Chemistry
University of Almeria
Almería, Spain
Carlos Goncalves
Interdisciplinary Centre of Marine and Environmental Research (CIIMAR/CIMAR)
University of Porto Porto, Portugal
Arnab Goon
National Referral Laboratory
ICAR-National Research Centre for Grapes Pune, India
Horacio Heinzen
Grupo de Análisis de Contaminantes Traza (GACT)
Departamento de Química del Litoral
Centro Universitario Regional (CENUR)
Litoral Norte and
Grupo de Análisis de Contaminantes Traza (GACT) Pharmacognosy
Facultad de Quimica
Universidad de la República (UdelaR) Montevideo, Uruguay
Ana Lozano
European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables (EURL-F&V)
Agrifood Campus of International Excellence (ceiA3)
Department of Physics and Chemistry
University of Almeria Almería, Spain
Paula Medina-Pastor
European Food Safety Authority, Pesticide Unit Parma, Italy
Antonio Molina-Díaz
Analytical Chemistry Research Group
Department of Physical and Analytical Chemistry
University of Jaén Jaén, Spain
Basil K. Munjanja
Department of Chemistry
University of Pretoria Pretoria, South Africa
Silvina Niell
Grupo de Análisis de Contaminantes
Traza (GACT)
Departamento de Química del Litoral
Centro Universitario Regional (CENUR)
Litoral Norte
Universidad de la República (UdelaR) Montevideo, Uruguay
Leo M.L. Nollet
Retired
University College Ghent Ghent, Belgium
Dasharath Oulkar
National Referral Laboratory ICAR-National Research Centre for Grapes Pune, India
Lucia Pareja
Departamento de Química del Litoral
Centro Universitario de Paysandú Universidad de la República Paysandú, Uruguay
Patricia Pérez-Ortega
Analytical Chemistry Research Group
Department of Physical and Analytical Chemistry
University of Jaén Jaén, Spain
Andrés Pérez-Parada Grupo de Materiales y Estudios Ambientales (GDMEA) and Grupo de Análisis de Compuestos Traza (GACT)
Universidad de la República (UdelaR) Montevideo, Uruguay
Łukasz Rajski
European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables (EURL-F&V)
Agrifood Campus of International Excellence (ceiA3)
Department of Physics and Chemistry
University of Almeria Almería, Spain
Chris Sack
U.S. Food and Drug Administration College Park, Maryland, USA
Vasilios G. Samaras
Water and Air Quality Laboratory
Department of Environment University of the Aegean Mytilene, Greece
Maria Augusta D. Sousa
Faculty of Pharmacy University of Porto Porto, Portugal
Stanisław Walorczyk
Department of Pesticide Residue Research Institute of Plant Protection–National Research Institute Pozna ń , Poland
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Section i Regulatory Issues
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1.2
Chapter 1 European Union Monitoring Programs
Paula Medina-Pastor
CONTENTS
The European Union (EU) monitoring programs consist of official controls that enforce the compliance of diverse aspects of the regulations in place. This chapter aims to clarify what an official control consists of, who plans them, what characteristics they have, who carries them out, what is the data collected used for, and other information. The first thing is to understand the legal frame in which they lay.
1.1 LEGAL FRAME
In order to afford EU citizens a high level of human, animal, and plant health and guarantee the functioning of the internal market, EU legislation provides for a set of harmonized rules to prevent, eliminate, or reduce the level of health risk to humans, animals, and plants, which may arise along the “agri-food chain” and the rules which ensure that it is safe and fit for human consumption. It also includes rules referred to as veterinary and phytosanitary legislation, which deal with risks to animal health and plant health in general, aiming to ensure the provision of information to consumers and to guarantee fair commercial practices in agri-food chain products’ trade. To ensure that this extensive set of rules is enforced by the Member States (MS) across the EU in a harmonized manner, a legislative framework of regulations has been established.
1.1.1 Regulation (EC) No. 882/2004
Regulation (EC) No. 882/20041 establishes a harmonized framework of general rules for the organization of official controls at the European level. The purpose of the official controls is that the EU MS enforce feed and food law, animal health and welfare, and monitor and verify that the relevant requirements are fulfilled by business operators at all stages of production, processing, and distribution. In order to have a global and uniform approach with regard to official controls, MS should establish and implement multiannual national control plans in accordance with broad guidelines drawn up at EU level. These guidelines should promote coherent national strategies and identify risk-based priorities and the most effective control procedures. The multiannual national control, once planned, establishes a solid basis for the Commission inspection services to carry out controls in the MS. The control plans enable the Commission to verify whether the official controls in the MS are organized in accordance with Regulation (EC) No. 882/2004 and are appropriate and, in particular, where the audit of the MS against the multiannual national control plans shows weaknesses or failures.
The frequency of official controls should be regular and proportionate to the risk, taking into account the results of the checks carried out by feed and food business operators in each MS. Ad hoc controls should be carried out at any time, more in the case of suspicion of noncompliance.
Multiannual national control plans are specifically contemplated under Article 41 and Article 42 of this Regulation stating the need of each MS to prepare a single integrated multiannual national control plan. The principles for the preparation are that since 2007, MS are having multiannual controls, regularly updated in the light of developments and providing the Commission with the latest version of the plan on request.
Each multiannual national control plan shall contain general information on the structure and organization of the systems of feed and food control and of animal health and animal welfare control in the MS concerned. In particular on the strategic objectives of the plan and on how the prioritization of controls and allocation of resources reflect these objectives; the risk categorization of the activities concerned; the designation of competent authorities and their tasks at central, regional, and local level and on resources available to these authorities; the general organization and management of official controls at national, regional, and local level, including official controls in individual establishments; control systems applied to different sectors and coordination between the different services of competent authorities responsible for official controls in these sectors; the delegation of tasks to control bodies; methods to ensure compliance with the operational criteria; the training of staff performing official controls; the documented procedures; the organization and operation of contingency plans for animal or food-borne disease emergencies, feed and food contamination incidents, and other human health risks and the organization of cooperation and mutual assistance.
The multiannual national control plans may be adjusted during their implementation. Amendments may be made in the light of, or in order to take account of, factors including new legislation; the emergence of new diseases or other health risks; significant changes to the structure, management, or operation of the competent national authorities; the results of MS’ official controls; scientific findings; and the outcome of audits performed by a third country in a MS.
European legislation is characterized by being active and applicable. Therefore, it is revised and updated every 10 years. For this reason, at the time of writing this chapter, Regulation (EC) No. 882/2004 is being amended. The outcome of the revised legislation aims to modernize and integrate the system of official controls in a manner that consistently accompanies the upgrade of EU policies in these sectors simplifying and clarifying the legislative framework such as eliminating redundant requirements (e.g., separate reporting from official controls on residues of veterinary medicinal products), allowing a proportionate and flexible approach to some specific situations (e.g., not requiring full accreditation of official laboratories in case of emergencies), or ensuring the availability of stable and appropriate resources, ensuring equity and fairness in the financing of official controls, and improving transparency to ensure the correct enforcement of the legislation.
1.1.2 Regulation (EC) No. 396/2005
The previous Regulation (EC) No. 882/2004 is a general food law. For the specific field of food and feed of plant and animal origin, Regulation (EC) No. 396/20052 was adopted. The adoption of this later Regulation on September 1, 2008, aimed at the harmonization of the maximum residue levels (MRLs). Before, each EU MS had its own MRL, 3–6 but in the interests of clarity and simplicity, those directives were repealed and replaced by a single act of this Regulation.
The Regulation directly concerns public health and is relevant to the functioning of the internal market, which, before, with different national MRLs for pesticides, posed barriers to trade of food products where MRLs could be different in different MS. These food products constitute Annex I of this Regulation. As a life system, Annex I of this Regulation was deeply revised,7 allowing a better understanding and reporting of the food products consumed in the EU which are not only produced but often imported. In the interest of free movement of goods, equal competition conditions among the MS, as well as a high level of consumer protection, MRLs for products of plant and animal origin are set at EU level, taking into account good agricultural practice.
It is important to protect plants and plant products against harmful organisms in order to prevent a reduction in yield or damage to them and to ensure both the quality of the products harvested and high agricultural productivity. For this reason, plant protection products are used to protect plants and plant products from the effects of harmful organisms. However, a possible consequence of their use may be the presence of residues in the treated products, in animals feeding on those products, and in honey produced by bees exposed to those substances. According to Regulation 1107/20098 (previous Directive 91/4149) concerning the placing of plant protection products on the market, public health needed to be given priority over the interests of crop protection, ensuring that such residues should not be present at levels presenting an unacceptable risk to humans and, where relevant, to animals. Therefore, MRLs are to be set at the lowest achievable level consistent with good agricultural practice for each pesticide with a view to protecting vulnerable groups such as children and the unborn. The MRLs are set in Annexes II and III of the Regulation and they are being revised permanently.
The residues of active substances in products of plant and animal origin arising from unauthorized use, environmental contamination, or from the use in third countries* should be carefully controlled and monitored due to the high level of imports.
MRLs for pesticides should be continually monitored and should be changed to take account of new information and data. MRLs should be set at the lower level of analytical determination where authorized uses of plant protection products do not result in detectable levels of pesticide residues. Where uses of pesticides are not authorized at EU level, MRLs should be set at an appropriately low level to protect the consumer from the intake of unauthorized or excessive levels of pesticide residues. In order to facilitate control of residues of pesticides, a default value is set for pesticide residues present in products or groups of products covered by Annex I of Regulation (EC) 396/2005, for which no MRLs have been established in Annexes II or III, unless the active substance in question is listed in Annex IV (annex that lists substances for which no MRL is required). The default value is set at 0.01 mg/kg and may be set at a different level for active substances covered by Annex V, taking into account the routine analytical methods available and/ or consumer protection.
The lifetime exposure and, where appropriate, the acute exposure of consumers to pesticide residues via food products are evaluated in accordance with EU procedures and practices, taking account of guidelines published by the World Health Organization.
To set MRLs, monitoring data might be used in particular for unauthorized pesticides that may be present in the environment. Through the World Trade Organization, the Union’s trading partners should be consulted about the MRLs proposed, and their observations are taken into account before the MRLs are adopted. MRLs set at the international level by the Codex Alimentarius Commission should also be considered when EU MRLs are being set, taking into account the corresponding good agricultural practices.
For food and feed produced outside the EU, different agricultural practices with regard to the use of plant protection products may be legally applied, sometimes resulting in pesticide residues differing from those resulting from uses legally applied in the EU. It is therefore appropriate that MRLs are set for imported products that take these uses and the resulting residues into account provided that the safety of the products can be demonstrated using the same criteria as for domestic produce.
It is the European Food Safety Authority (EFSA) who assess the MRL applications and evaluation reports prepared by the MS, taking into account the full range of toxicological effects such as immunotoxicity, endocrine disruption, and developmental toxicity, with a view to determining the associated risks to consumers and, where relevant, to animals.
This Regulation establishes MRLs for the control of pesticide residues in food and feed and recommends MS to establish national programs to control these residues. The results of the national control programs are to be submitted to the Commission, the EFSA, and the other MS and are included in the EU Annual Report published annually by EFSA.
To ensure that consumers are kept adequately informed, MS publish their results of the national monitoring residues annually on the Internet, providing all individual data, including the place of collection.
* The EU refers to first, second, and third countries referring to the distance from them, therefore MS are first countries, EFTA countries are second countries, and the rest of the countries are third countries.
FIGURE 1.1 Schema of the different parts involved in the EU monitoring system.
Under this Regulation, MS carry out official controls on pesticide residues in order to enforce compliance with the legal Maximum Residue Limit and also to assess risk based consumption on the European food diet.
1.1.3
Regulation (EC) No. 178/2002
Regulation (EC) No. 178/200210 lays down the procedures in matters of food law and establishing the EFSA. The EFSA assesses and communicates on all risks associated with the food chain. Frequently, advice is given to support the risk management and policymaking processes. These may involve the process of adopting or revising European legislation on food or feed safety, deciding whether to approve regulated substances such as pesticides or developing new regulatory frameworks and policies. The EFSA gives independent advice based on a solid scientific foundation, aiming to provide appropriate, consistent, accurate, and timely communications on food safety issues to all stakeholders and the public in general, based on risk assessments and scientific expertise.
Overall, the different parts involved in the EU monitoring programs are those mentioned in the EU legislation frame, and its interactions are shown in Figure 1.1. All parts work for the common objective of providing safe food to the European consumer.
1.2
OFFICIAL CONTROLS
In the field of pesticides, there are in place two types of official control programs.
1.2.1
EU-Coordinated Multiannual Control Program (EUCP)
The European Commission prepares the EU-coordinated multiannual control program (EUCP), as it is stated in Regulation (EC) 396/2005, identifies specific samples to be included and takes into account problems that have been identified regarding compliance
with MRLs, with a view to assess consumer exposure and the application of the legislation in place. It is programmed for a three-year cycle but in general is adopted and updated every year. A draft of this program is presented to the Standing Committee at least six months before the end of each calendar year. It is commonly known as the “EU-coordinated multiannual programme.” It aims to provide statistically representative data regarding pesticide residues in food available to European consumers defining the food products and pesticides that should be monitored by MS. Table 1.1 summarizes the latest regulations concerning the coordinated multiannual program of the EU.
Annex I of each of the EU-coordinated multiannual program regulations lists the pesticides to be monitored. The Regulation is set to a three-year cycle; i.e., 2009 and 2012 may be compared. It is normally revised and republished with amendments. If substances to be monitored are changed, it will apply to the third year cycle. The evolution in the last six years of the pesticide scope requested in the Regulations can be seen in Table 1.2. On a yearly basis, the MS, European Commission, and EFSA join to discuss the inclusion or exclusion of pesticides in the forthcoming program. The decision of including new pesticides is based on, e.g., EFSA suggestions based on the findings reported by MS from the previous years. It can also be the MS suggestions based on the notifications of the Rapid Alert System for Food and Feed (RASFF).11 The RASFF system is set on Article 50 of Regulation (EC) No. 178/2002. It is a harmonized notification system aimed to ensure an effective communication between MS contact points, the national competent authorities, and the Commission. Each MS is responsible in its jurisdiction for exchanging information with other MS about measures taken in response to serious risks identified in relation to food or feed. The information exchange facilitates a more rapid and coordinated response by MS to a health threat. The network includes the MS, the EFSA, and the European Commission, as member and manager of the system. Switzerland and the European Economic Area countries are also involved.
Pesticides might also be taken out of the program because there are no findings reported over the years (e.g., cadusafos or campheclor have not been further monitored since 2011). Moreover, it is the responsibility of the competent authorities in each MS to follow the corresponding legal residue definition according to the food product that is analyzed. For instance, the residue definition followed for “boscalid” will be “boscalid as parent compound” for food products of fruit, vegetable, or cereal origin, whereas for animal origin food, the residue definition to be followed should be “sum of boscalid and M 510F01 including its conjugates.” Not following a complete residue definition will hamper the checks for enforcement and the quality of the results itself. The consultation of the residue definition in place at the time of the analysis is carried out and can be checked on the EU Pesticide Database,12 although the legal definitions are those published in the Official Journal of the European Union.13 The residue definitions might change after the MRL has been revised and a corresponding Reasoned Opinion is published by EFSA. The scientific work produced by EFSA is taken into account by the European Commission and it is later voted among the MS in the Standing Committee on Plant, Animal, Food, and Feed. The EU-coordinated monitoring regulations normally mention the parent compound. It is the competent Authority that checks the residue definition that applies to that compound and if analysis of further substances is needed (e.g., by aldicarb: aldicarb sulfone and aldicarb sulfoxide should also be analyzed; by malathion: malaoxon should also be analyzed). This allows the MSs to be aware of the need to completely follow the residue definition (e.g., dimethoate and omethoate, methomyl and thiodicarb, triadimenol and triadimefon).
The EU-coordinated program requests not only a certain number of pesticides to be analyzed but also a certain number of food products to be collected on which the
TABLE 1.1
Summary of the Latest EU Coordinated Program Regulations
Regulation Year of Application
Regulation (EC) no. 1213/2008
Regulation (EC) no. 901/2009
2009
Regulation (EU) no. 915/2010
2010
Regulation (EU) no. 1274/2011
2011
Regulation (EU) no. 788/2012
2012
2013
Reference
Commission Regulation (EC) no. 1213/2008 of 5 December 2008 concerning a coordinated multiannual community control program for 2009, 2010, and 2011 to ensure compliance with maximum levels of and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin.
OJ L 328, 6.12.2008, p. 9–17.
Commission Regulation (EC) no. 901/2009 of 28 September 2009 concerning a coordinated multiannual community control program for 2010, 2011, and 2012 to ensure compliance with maximum levels of and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin.
OJ L 256, 29.9.2009, p. 14–22.
Commission Regulation (EU) no. 915/2010 of 12 October 2010 concerning a coordinated multiannual control program of the Union for 2011, 2012, and 2013 to ensure compliance with maximum levels of and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin.
OJ L 269, 13.10.2010, p. 8–18.
Commission Implementing Regulation (EU) no. 1274/2011 of 7 December 2011 concerning a coordinated multiannual control program of the Union for 2012, 2013, and 2014 to ensure compliance with maximum residue levels of pesticides and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin.
OJ L 325, 8.12.2011, p. 24–43.
Commission Implementing Regulation (EU) no. 788/2012 of 31 August 2012 concerning a coordinated multiannual control programme of the Union for 2013, 2014, and 2015 to ensure compliance with maximum residue levels of pesticides and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin.
OJ L 235, 1.9.2012, p. 8–27.
Regulation (EU) no. 788/2012 2014 No new regulation was published.
Regulation (EU) no. 400/2014
2015
Commission Implementing Regulation (EU) no. 400/2014 of 22 April 2014 concerning a coordinated multiannual control program of the Union for 2015, 2016, and 2017 to ensure compliance with maximum residue levels of pesticides and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin.
OJ L 119, 23.04.2014, p. 44–56.
TABLE 1.2 Pesticides Requested in the EU Coordinated Program between the Years 2009 and 2015
Pesticides Requested
2,4-D
Abamectin
Acephate
Acetamiprid
Acrinathrin
Aldicarb
Azinphos-methyl
Azoxystrobin
Benfuracarb
Bifenthrin
Biphenyl
Bitertanol
Bixafen
Boscalid
Buprofezin
Cadusafos
Campheclor
Carbendazim
Carbofuran
Carbosulfan
Chlorantraniliprole
Chlorfenapyr
Chlorfenvinphos
Chlormequat
Chlorobenzilate
Chlorothalonil
Chlorpropham
Chlorpyrifos
(Continued)
TABLE 1.2 (CONTINUED) Pesticides Requested in the EU Coordinated Program between the Years 2009 and 2015
Pesticides Requested in the EUCP
Chlorpyrifos-methyl
Clofentezine
Clothianidin
Cyfluthrin
Cymoxanil
Cypermethrin
Cyproconazole
Cyprodinil
Cyromazine
Deltamethrin
Dichlofluanid
Dichlorvos
Dicloran
Dicofol
Dicrotophos
Diethofencarb
Diflubenzuron
Diniconazole
Dinocap
Diphenylamine
Dithianon
Dithiocarbamates
Dodine
Endosulfan
Ethephon
Ethirimol
Ethoprophos
Etofenprox
Famoxadone
(Continued)
TABLE 1.2 (CONTINUED) Pesticides Requested in the EU Coordinated Program between the Years 2009 and 2015
Pesticides Requested
Fenamidone
Fenamiphos
Fenarimol
Fenazaquin
Fenbuconazole
Fenhexamid
Fenitrothion
Fenpropidin
Fenpropimorph
Fenpyroximate
Fenthion
Fenvalerate
Fipronil
Flonicamid
Formetanate
Formothion
Fosthiazate
Glyphosate
Heptachlor
Hexachlorocyclohexane (alpha)
Hexachlorocyclohexane (beta)
Hexaconazole
Hexythiazox
Imazalil
Imidacloprid
(Continued)
TABLE 1.2 (CONTINUED) Pesticides Requested in the EU Coordinated Program between the Years 2009 and 2015
Pesticides Requested in the EUCP
Indoxacarb
Ioxynil
Iprodione
Iprovalicarb
Isocarbophos
Isofenphos-methyl
Isoprocarb
Isoprothiolane
Kresoxim-methyl
Mepanipyrim
Mepiquat
Meptyldinocap
Methoxyfenozide
Metobromuron
Monocrotophos
Myclobutanil
TABLE 1.2 (CONTINUED) Pesticides Requested in the EU Coordinated Program between the Years 2009 and 2015
Pesticides Requested
Pencycuron
Pendimethalin
Permethrin
Phenthoate
Phosalone
Phosmet
Phoxim
Pirimiphos-methyl
Procymidone
Profenofos
Propamocarb
Propargite
Propiconazole
Propoxur
Propyzamide
Prothioconazole-desthio
Prothiofos
Pymetrozine
Pyraclostrobin
Pyrethrins
Pyridaben
Pyrimethanil
Pyriproxyfen
Quinoxyfen
Quintozene
Resmethrin
Rotenone
Spinosad
Spirodiclofen
Spiromesifen
Spiroxamine
Tecnazene
(Continued)
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ONNI.
Maa liian kaunis, taivas liian kirkas on, sen sini liian väkevä ja polttavainen. Maan lapselle on armo ansaitsematon, jo täällä saada onni, autuus taivahainen.
Kuin jäinen puu, mi alastonna raukenee
tuoll' alttihiksi kevätpäivän syleilylle, niin sieluni mun asunnoksi aukenee nyt ilolle, ah, ikävöiden itketylle.
Kuink' onkaan suurin ihme yksinkertainen! Vain haaveksia, rukoella hartahasti, niin saapuu kaikki myötä hetken ainoisen, ja malja kallis täyttyy kukkuroilleen asti.
Elämän riemu katsoo silmin palavin, ne polttavat niin syvän, taivaan siintävinä.
Mit' ikävöisin enää, mitä kaipaisin?
Jo tulin liian, liian rikkahaksi minä.
ME KAKSI VALKOISTA LINTUA —
Me kaksi valkoista lintua nyt lennämme pilvien taa. Niin kauas, niin kauas jää allemme pieni maa. Me raikkaita tuulia halkoen nyt uimme avaruutehen, ja huikaisun meri soi ympäri, suonissa humisee veri. Me sineä juomme riemusta humaltuen.
Me kaksi valkoista lintua nyt lennosta väsähtäin alas syöksymme pyörtyin kautt' ilmojen häikäiseväin. Kaks ruumista maassa värisee, sydän sydäntä vasten kylmenee. Kylän pienokaiset ne laulaen pitävät hautajaiset, laps'äänet heleät yllämme helkkyilee.
Me kaksi valkoista lintua nyt varjossa pähkinäpuun unt' onnesta näämme ja tuoksuista toukokuun. Sinivuokot kummulla kukkivat, ja ylhäältä pilvenhattarat niin hauraina hymyy … Ah, sinne sinisyyksihin lymyy ilon ihanin hurma ja haaveet puhtaimmat.
HELLUNTAIKELLOT.
Halki aamun terhenen soi ääni armahani. Herään — soivat huomenkellot kautta ikkunani.
Kuinka sentään ihanaa on ihmislapsen elää! Sävel elon suuren laulun suonissani helää — suonissani soiden helää ilo, kaiho verten nuorten. Oi, jos kelloin kaiku kantais minut kauas yli laaksoin, vuorten —!
VALKEA PÄIVÄ.
Ajatukseni lailla auringon säteen säihkyy, karkeloi. Sinä, ken ani armaasti tartuit käteen, kuuntele, kuuntele, kuinka mun syömeni soi!
On kuin joku jouhisoittimehen siellä kajoais, kiviraunion karuun tummuutehen valkea pensas luntansa varistais.
Suvilämminnä siintää taivaan kaari yllä kaupungin. Tule, jossain on tuoksuva jasmiinisaari, linna ja portaat, johtavat pilvihin!
Taivas, pilvien anna ratketa itkemähän! Pieni sydän pakahtuupi autuuteensa tähän.
PILVINEN PÄIVÄ.
Rannalta kurjenmiekkoja poimin ja kuuntelen kuikan ääntä.
Miksi nyt niin tuulessa valittavat kaislat ja pilveen on peittynyt taivas?
Eikö eilen kurjenmiekat aurinkoa juoneet ja nurmi ollut houkuttavan lämmin?
Eikö mua kutsunut hän nurmilinnuksensa, kun poveansa vasten minut painoi?
Pilvipäivät saavat, ah, aurinkoisten jälkeen, kun huikaisevan kirkasta on ollut! —
Pääskyset jo liitelevät alahalla aivan, ja apea on kuikan ääni.
ORJANRUUSU.
Mua kutsuu metsäsaari pois vainioiden taa. Käyn sinne kesäyönä, kun kaste kimaltaa.
Ma karhunsammalmättäälle vaivun itkemään, ja kyyneleeni virtaa maan multaan viileään.
Ah, orjanruusupensas mun oli rakkautein!
Sen oksat sormin vertyvin seppeleeksi tein.
Ja kukkaterät puunsi kuin sisus kirsikan, mut joka piikki myötään toi kivun katkeran.
Nyt polkeako täytyy mun ruusut rakkautein, suur ikävä ja riemu ja tuska sydämein?
Oi lausu itse, armas, sun kuinka kieltää voin, kun silmiesi loisteen ma sieluhuni join!
Oi lausu itse, kuinka sun poistan muistostain, kun läsnäolos autuuden tuntea ma sain, kun öin ja päivin äänes mun korvissani soi…
Ah, liian paljon lemmin, sua unhottaa en voi!
SCHUMANNIN »TRÄUMEREI».
On ilma kellanhimmeä — se tuoksuu jasmiinilta, ja lyhdyt tanssipaviljonkiin heittää säihkettään. Mut huvilasta, korkealta köynnösterassilta soi sellon tumma ääni yksinään. On ilma kellanhimmeä — se tuoksuu jasmiinilta… — Mun joku pyytää soutelemaan venheellään.
Yö samettinen, lämmin, vedenpinta peilityyni, kuin sulaa kristallia venhe hiljaa halkoilee. Oon soutajasta haaveksinut salaa — tunnen syyni: kuin pieni lintu sydän vapisee. Yö samettinen, lämmin, vedenpinta peilityyni… — Jo sellon syvä, tumma ääni vaikenee.
DOLCE FAR NIENTE.
On alla auringon heleän
niin lämmin rinteellä maata mäen.
Ma kuulen hyttysten hyrinän ja muurahaisten ma saatot näen.
On olo rauhaa ja unelmaa.
Näin oman sykkeensä sydän kuulee.
Nyt toistaan lempivät taivas, maa.
Vain metsäsaarelta salaa tuulee.
Kuin kimalainen, mi laskeuu
tuon kelta-angervon kukinnolle, niin olen ahnas ja herkkusuu ma kesän tuoksulle, auringolle.
V.Jo täynnä kennot on hunajaa, ja uutta tuo joka uusi huomen. Ah, autuaasti mua unettaa. Se painaa umpehen silmäluomen.
OCEANIA.
(à la Pierre Loti). Maa merellinen kookospalmuines, yöperhoines — ma poimimaan käyn koralleja rannoilles.
Sa mitään muista, mitään toivo et.
Sa mieti et.
Vain valtameren hengitystä kuuntelet.
Ja Tyynimeri suolavuoteellaan sun autuaan, sun onnellisen suutelee yön unholaan, kun yli basalttisen louhikon lyö vallaton veen hyöky. Valkojasmiinis kuin vaahto on.
Ei laula ykskään pieni siivekäs
sun metsissäs, vain kaiku vastaa varjoisista siimeistäs,
laps aaltojen ja aavistusten maan
kun kaipuutaan
yön hiljaisuuteen huhuu ruokohuilullaan.
FANTASIA.
Jossain pyörryttävän kaukana — öljytyynen, kavalan valtameren villin rehevässä saaressa kelluu hunajankeltainen jättiläiskukka höyryävän lammen pinnalla niinkuin oudon suuri, samettinen dahlia —
Loistavat, myrkylliset hyönteiset laskevat miljoonia muniaan limantahmeiden terälehtien lomiin. Metsän kuumehorteisista puista tippuu helmeilevä tuskanhiki jossain pyörryttävän kaukana —
MYRKKYLILJAT.
Voi häntä, jolle nykyisyys ei riitä! Hän vaatii myöskin ajan mennehen ja poimii niinkuin polttoyrtit siitä jok' ainoon lemmittynsä askelen.
Hän suven hyvää hedelmää ei niitä, hän myrkyttämä mustain liljojen. Hän saamastaan ei sallimusta kiitä, vaan itkee maata, joka vajos merehen!
Ah, kesken suudelmia suruun vaipuin voi värähdellä mimosan hän lailla ja vaiti on, ei nosta katsettaan.
Kuut kauniit katoo kyynelusviin haipuin, ja unen lempeätä lahjaa vailla hän öisin vääntelehtii vuoteellaan.
MUSTANPUNAINEN MELANKOLIA.
Kookospalmujen siimestämä tie, jota käyden askeleeni kantaa pitkin ahnaan, huohottavan meren liejuista rantaa.
Luode kaikki rakkaimpani vie, muodottomia ruumiita mukanaan vuoksi kantaa.
Kookospalmujen siimestämä tie, tumma loimu aarniometsäin yllä raskas murhe sydämessä hyljätyllä.
Mikä tähti palanutkaan lie kerran unikoilla peitetyn kehtoni yllä?
Kuuma, vereen kastettu tähti paloi!
ODALISKI.
Hän lojuu pieluksilla divaanin, ja olkapäältä liukuu silkkihiha. On huulet punaiset kuin luumun liha, mut kasvot kuultaa lailla balsamin.
Ja ikkunansa peittyin ruusuihin kuin hiillos hehkuu silmissään on viha: ei riitä niille puisto, pylväspiha, ne köynnösverkoin kietoo seraljin.
Niin tukehduttaa lemu myrhan, myskin, ja unhottunut ilmain heleyskin on tällä puolen tumman ristikon.
Ah, siellä virta välkkyy auringossa, ja täysin purjein keinuu aallokossa nyt laiva lähtövalmis, levoton —!
LOTI AZIYADÉLLE.
Oi Sirkassian metsien myrttikukka, joka suot minun juoda huultesi hunajaa!
Sinä suloinen! Syvin lainein aaltoaa alas olkapäillesi ambrantuoksuinen, tumma tukka.
Aziyadé!
Valot kirkkaat illoin syttyvät Stambulissa, väri silmäisi fosforiloistein kimmeltää.
Sisin sielus arvoitukseksi aina jää, sinä Aasian poloinen, silkinpehmeä pieni kissa.
Aziyadé!
KEVÄISET AROT.
Tuulen siivin lempi toi mun halki aromaan. Kukkaverho kirjava sen peitti kokonaan. —
Nauratko, kaunis Katinka?
Kukkasiksi muuttua jos onnemme nyt vois, tuoksuavan tulvan alla laajat arot ois! — Uskotko, armas Katinka?
Lauloi nuori gondolieri hämyssä Venetsian yön: itkettävää niin ei ole mitään kuin on kylmä, lemmetön syön!
Sulaa vuorten sininen jääkin, ei sula sydämesi sun, säihkyvän ihana, julma Judith, riistäjä rauhani, toivoni mun!
Kukkivat visaiset viikunapuutkin, lempeen ei puhkea lemmetön syön! Hiljaa kapea gondooli liukui hämyssä Venetsian yön.
RAKKAUS.
Ruusu puhkesi punainen keskellä keltaista poutaa. Tumma, polttava viini sen suonissa soi ja soutaa. Pisaran yhden jos viiniä juo ikuinen onni vuottaa, kaksi pisarta tuskan tuo, kolme kuoleman tuottaa.
