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PESTICIDES ͳ STRATEGIES FOR PESTICIDES ANALYSIS Edited by Margarita Stoytcheva Pesticides - Strategies for Pesticides Analysis Edited by Margarita Stoytcheva Published by InTech Janeza Trdine 9, 51000 Rijeka, Croatia Copyright © 2011 InTech All chapters are Open Access articles distributed under the Creative Commons Non Commercial Share Alike Attribution 3.0 license, which permits to copy, distribute, transmit, and adapt the work in any medium, so long as the original work is properly cited. After this work has been published by InTech, authors have the right to republish it, in whole or part, in any publication of which they are the author, and to make other personal use of the work. Any republication, referencing or personal use of the work must explicitly identify the original source. Statements and opinions expressed in the chapters are these of the individual contributors and not necessarily those of the editors or publisher. No responsibility is accepted for the accuracy of information contained in the published articles. The publisher assumes no responsibility for any damage or injury to persons or property arising out of the use of any materials, instructions, methods or ideas contained in the book. Publishing Process Manager Iva Lipovic Technical Editor Teodora Smiljanic Cover Designer Martina Sirotic Image Copyright Olivier Le Queinec, 2010. Used under license from Shutterstock.com First published January, 2011 Printed in India A free online edition of this book is available at www.intechopen.com Additional hard copies can be obtained from orders@intechweb.org Pesticides - Strategies for Pesticides Analysis, Edited by Margarita Stoytcheva p. cm. ISBN 978-953-307-460-3 free online editions of InTech Books and Journals can be found at www.intechopen.com Contents Preface Chapter 1 Chapter 2 IX Current Trends in Liquid-Liquid Microextraction for Analysis of Pesticide Residues in Food and Water Sara C. Cunha, J.O. Fernandes and M. Beatriz P.P. Oliveira Sample Preparation in the Analysis of Pesticides Residue in Food by Chromatographic Techniques Guan Huat Tan and Mee-Kin Chai Chapter 3 Analytical Methods for Viable and Rapid Determination of Organochlorine Pesticides in Water and Soil Samples 59 Senar Ozcan, Ali Tor and Mehmet Emin Aydin Chapter 4 Factors Affecting the Accurate Quantification of Pesticide Residues in Non-Fatty Matrices 83 Panagiotis Georgakopoulos and Panagiotis Skandamis Chapter 5 Chemical Analysis of Pesticides Using GC/MS, GC/MS/MS, and LC/MS/MS Renata Raina 1 27 105 Chapter 6 Fast Gas Chromatography and Its Use in Pesticide Residues Analysis 131 Svetlana Hrouzková and Eva Matisová Chapter 7 Multidimensional Chromatography in Pesticides Analysis 155 Tomasz Tuzimski Chapter 8 Rapid and Easy Multiresidue Method for Determination of Pesticide Residues in Foods Using Gas or Liquid Chromatography–Tandem Mass Spectrometry 197 Satoshi Takatori, Masahiro Okihashi, Yoko Kitagawa, Naoki Fukui, You Kakimoto-Okamoto and Hirotaka Obana VI Contents Chapter 9 Organochlorine Pesticides in Human Serum Jung-Ho Kang and Yoon-Seok Chang Chapter 10 Urea Pesticides 241 Simone Morais, Manuela Correia, Valentina Domingues and Cristina Delerue-Matos Chapter 11 Liquid Chromatography in Studying Lipophylicity and Bioactivity of Pesticides 263 Małgorzata Janicka Chapter 12 Pesticide Immunoassay 293 Mingtao Fan and Jiang He Chapter 13 Organophosphorous CompoundsToxicity and Detection Approach 315 Sanjay Upadhyay, Mukesh K. Sharma, Vepa K. Rao, Bijoy K. Bhattacharya, Dileep Sharda and R.Vijayaraghavan Chapter 14 New Materials in Electrochemical Sensors for Pesticides Monitoring 333 M. Aránzazu Goicolea, Alberto Gómez-Caballero and Ramón J. Barrio Chapter 15 Organophosphorus Pesticides Determination by Electrochemical Biosensors 359 Margarita Stoytcheva, Roumen Zlatev, Zdravka Velkova, and Benjamin Valdez Chapter 16 Mercaptobenzothiazole-on-Gold Organic Phase Biosensor Systems: 4. Effect of Organic Solvents on Organophosphate and Carbamate Pesticide Determination 373 V. Somerset, P. Baker and E. Iwuoha Chapter 17 An analytical Task: A miniaturized and Portable µConductometer as a Tool for Detection of Pesticides 387 Libuse Trnkova, Jaromir Hubalek, Vojtech Adam and Rene Kizek 215 Preface The synthesis, during the 1950s, of organophosphorus, carbamate, organochlorine, and pyrethroid compounds, designed for preventing, destroying, repelling or mitigating any pest, marked the beginning of the contemporary “pesticides era”. Users’ benefits, because of the successful pesticides application for parasites control of field and fruit crops leading to an increase of the agricultural production, became evident. However, pesticides toxicity and indiscriminate usage caused risks to men and his environment. Therefore, the World Health Organization (WHO), the Food and Agricultural Organization of the United Nations (FAO), the Codex Alimentarius Commission, the EU Commission, and the U. S. Environmental Protection Agency (EPA), among others, enacted the allowable pesticide residue levels in food, drinking water and environmental samples. The European Council Directive 98/83/EC on the quality of water intended for human consumption sets the limit value of the individual pesticides in drinking water at 0.1 g L-1 and of the total pesticides at 0.5 g L-1. According to the U.S. EPA Office of Ground Water and Drinking Water (OGWDW), the health advisory levels for some organophosphorus pesticides in drinking water are: diazinon 3 g L-1, parathion-methyl 2 g L-1, disulfoton 1 g L-1, fenamiphos 2 g L-1, etc. At this time, EPA is reassessing pesticide residue limits in food to ensure that they meet the safety standard established by the Food Quality Protection Act of 1996. The great public concern and the strict legislation incited the development of reliable, specific, selective and sensitive analytical methods for pesticides monitoring. This book presents some of them. The first four chapters focus on sample preparation required by the chromatographic pesticides analysis to eliminate interferences and to increase sensitivity. Chapter 1 discusses the current trends in liquid-liquid microextraction for analysis of pesticides residues in food and water. Chapter 2 comments on a number of extraction procedures, as liquid-liquid extraction, solid phase extraction, solid phase microextraction, single drop microextraction, liquid-solid microextraction, microwave assisted solvent extraction, supercritical fluid extraction, dispersive liquid-liquid microextraction and accelerated solvent extraction. Chapter 3 points out on the application of miniaturized ultrasonic extraction for residues analyses of organochlorine pesticides in water and soil samples. Chapter 4 considers factors affecting the accurate quantification of pesticide residues in non-fatty matrices, including effects due to solvent and other materials applied for the residues extraction from the analyzed matrix, molecule polarity, matrix chemical composition, etc. X Preface Chapters 5 to 11 are dedicated to the application of chromatographic techniques in pesticides analysis. Chapter 5 focuses on issues related to the chromatography-mass spectrometry and instrumental approaches to improve selectivity and sensitivity of the determinations. Selectivity enhancement by the negative chemical ionization approach is commented in Chapter 6. Applicability of fast GC for pesticide residues in real-life samples is demonstrated, too. Chapter 7 introduces the principles of the multidimensional chromatography applied in pesticides analyses. In Chapter 8 the authors describe their “rapid and easy” multiresidue methods for determination of pesticide residues in food using gas or liquid chromatography-tandem mass spectrometry. Chapter 9 recommends the continuous human biomonitoring of organochlorine pesticides used in human serum isotope dilution gas chromatography-high-resolution mass spectrometric analysis. Analytical determination of urea pesticides is discussed in Chapter 10. Studying lypophilic properties and bioactivity of pesticides by liquid chromatography is the subject of Chapter 11. Chapters 12 and 13 address the immunoassay- and biosensors-based techniques for pesticides quantification. Chapter 14 is centered on the development of electrochemical sensors based on chemical or biological recognition processes and the advantages provided by nanomaterials electrode modification. Chapter 15 reviews the principles of the electrochemical biosensors-based methods for organophosphorus pesticides determination as methods of choice for “in situ” and “on line” application. The recent trends in the development of electrochemical biosensors, including nanomaterials transducer modification and genetic engineering of the biological recognition element are revised. Chapter 16 reports the results obtained by applying a gold-mercaptobenzothiazole-polyaniline-acetylcholinesterase-polyvinylacetate thick film amperometric biosensor for the detection of selected organophosphorus and carbamates pesticide in the nanomolar concentration range. Chapter 17 describes a miniaturized and portable new conductometer coupled with haloalkane dehalogenase, an enzyme able to cleave chlorinated chemicals, to detect pesticides applying a bipolar pulse technique. The book contains up-to-date publications of leading experts. It addresses the key problems in pesticide analysis related to the sample preparation techniques and the application of the current chromatographic and alternative biosensors-based methods. The references at the end of each chapter provide a starting point to acquire a deeper knowledge on the state of the art. The edition is intended to furnish valuable recent information to the professionals involved in pesticides analysis. Finally, it is my pleasant duty to acknowledge each of the authors for contributing their chapters to this volume. Margarita Stoytcheva Mexicali, Baja California Mexico