Pesticide Protocols Pesticide Protocols

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xiv Contributors JOHN PATSIAS • Aristotle Pesticide Science Laboratory, University of Thessaloniki, Thessaloniki, Greece JANUSZ PAWLISZYN • Department of Chemistry, University of Waterloo, Waterloo, Canada DOLORES PÉREZ-BENDITO • Department of Analytical Chemistry, Faculty of Sciences, University of Córdoba, Córdoba, Spain YOLANDA PICÓ • Laboratory of Bromatology and Toxicology, Faculty of Pharmacy, University of Valencia, Valencia, Spain JOSEANE M. POZZEBON • Departamento de Química Analítica, Instituto de Química, Universidade Estadual de Campinas, Campinas, SP, Brazil SONIA C. N. QUEIROZ • Laboratório de Dinâmica de Agroquímicos, Embrapa Meio Ambiente, Jaguariúna, SP, Brazil SARA RODRÍGUEZ-MOZAZ • Department of Analytical Chemistry, Faculty of Sciences, University of Córdoba, Córdoba, Spain SOLEDAD RUBIO • Department of Analytical Chemistry, Facultad De Ciencias, Edificio Anexo Marie Curie, Córdoba, Spain HASSAN SABIK • Food Research and Development Center, Agriculture and Agri-Food Canada, St-Hyacinthe, Quebec, Canada MITSUSHI SAKAMOTO • Tokushima Prefectural Institute of Public Health and Environmental Sciences, Tokushima, Japan GIANFRANCO SCIARRA • Unità Funzionale di Igiene Industriale e Tossicologia Occupazionale (Department of Industrial Hygiene and Occupational Toxicology) Laboratorio di Sanità Pubblica, Azienda USL 7 (Public Health Laboratory, National Health Service Local Unit 7), Siena, Italy CARLOS SONNENSCHEIN • Department of Anatomy and Cellular Biology, Tufts University School of Medicine, Boston, MA ANA M. SOTO • Department of Anatomy and Cellular Biology, Tufts University School of Medicine, Boston, MA MASAHIKO TAKINO • Yokogawa Analytical Systems Inc., Tokyo, Japan TAIZOU TSUTSUMI • Tokushima Prefectural Institute of Public Health and Environmental Sciences, Tokushima, Japan KATINKA E. VAN DER JAGT • TNO Chemistry, Food and Chemical Risk Analysis, Zeist, The Netherlands; currently, European Medicines Agency, London, UK JEANETTE M. VAN EMON • Methods Development and Research Branch, National Exposure Research Laboratory, US Environmental Protection Agency, Las Vegas, NV JOOP J. VAN HEMMEN • TNO Chemistry, Food and Chemical Risk Analysis, Zeist, The Netherlands ZISIS VRYZAS • Pesticide Science Laboratory, Aristotle University of Thessaloniki, Thessaloniki, Greece JI Y. ZHANG • GlaxoSmithKline, King of Prussia, PA
Endocrine Disrupter Pesticides by GC–MS/MS 3 1 Analysis of Endocrine Disruptor Pesticides in Adipose Tissue Using Gas Chromatography–Tandem Mass Spectrometry Assessment of the Uncertainty of the Method José L. Martínez Vidal, Antonia Garrido Frenich, Francisco J. Egea González, and Francisco J. Arrebola Liébanas Summary A multiresidue method based on extraction with organic solvents, cleanup by preparative liquid chromatography, and detection by gas chromatography (GC) using tandem mass spectrometry (MS/MS) mode is described for the determination of α- and β-endosulfan and three main metabolites (sulfate, ether, and lactone) in human adipose tissue samples. The analytical methodology is verified, and the values of some performance characteristics, such as linearity, limit of detection (LOD), limit of quantification (LOQ) limits, precision (intraday and interday), and accuracy (recovery) are calculated. The high efficiency of the cleanup step for the elimination of interference allows reaching detection limits at low micrograms per kilogram (parts per billion, ppb) concentration levels. In addition, an estimation of measurement uncertainty, using validation data, is presented for each target compound. The results show that the sources of largest uncertainty are those relative to the balance calibration, from the gravimetric step, and both the relative uncertainty associated with the recovery and the intermediate precision of the method. Key Words: Cleanup; endocrine disruptor; endosulfan; gas chromatography; metabolites; human adipose tissue; measurement uncertainty; organochlorine compounds; pesticides; preparative liquid chromatography; tandem mass spectrometry. 1. Introduction Organochlorine pesticides, such as endosulfan, are persistent environmental contaminants and tend to accumulate in humans and other animals (1,2). Endosulfan is still widely used in agricultural activities in developed countries because of its low relative persistence in comparison with other organochlorinated insecticides and its From: Methods in Biotechnology, Vol. 19, Pesticide Protocols Edited by: J. L. Martínez Vidal and A. Garrido Frenich © Humana Press Inc., Totowa, NJ 3
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OCPs in Human Fluids by SPDE and GC
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2,4-D and MCPA in Human Urine 91 7
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2,4-D and MCPA in Human Urine 93 4.
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2,4-D and MCPA in Human Urine 95 Ta
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118 Zhang 15. Crespin, M. A., Galle
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120 Knopp The search for alternativ
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HTS-IS-ELISA for Biomonitoring Chlo
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172 Glass questions that may arise
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Determination of Insecticides in In
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185 Fig. 3. Total ion current (TIC)
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Exposure to Malathion and Metabolit
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Internal Quality Criteria 219 17 Qu
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223 Fig. 1. Basic components of the
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Internal Quality Criteria 225 Fig.
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Pesticide Analysis by ELISA 231 18
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Pesticide Analysis by ELISA 233 4.
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QuEChERS Approach for Pesticides 23
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253 Table 2 Conditions for the GC-M
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Pesticide Analysis by LPGC-MS/MS 27
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286 Barker shorten turnaround time,
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320 Papadopoulou-Mourkidou, Papadak
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LC/LC for Pesticide Analysis 383 29
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Triazine in Water 467 34 Determinat
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Triazine in Water 477 (>60%) except
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Index 491 Index Adipose tissue anal
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Index 493 high-throughput screening
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Index 495 Food analysis, see Atrazi
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Index 497 HPLC, see High-performanc
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Index 499 quality control, 98 recov
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Index 501 Pyrethroids, air sampling
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Index 503 Uncertainty, estimation,
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