| Responsible Department | Department of Basic Science and Environment | ||||||||||||||
| Research School | Environmental Chemistry, Microbiology and Toxicology (RECETO) | ||||||||||||||
| Course Dates | Januar-Juni 2013 | ||||||||||||||
| Course Abstract | The aim of the course is for the student to be able to select the appropriate methods for extracting, cleaning up and measuring the very lipophillic insecticides, pyrethroids, and azole fungicides in environmental matrices such as water, sediment and animal tissue. The student should also be able to perform the analyses in practice. | ||||||||||||||
| Course Registration | Hos Nina Cedergreen | ||||||||||||||
| Deadline for Registration | 1/1 2013 | ||||||||||||||
| Credits | 7.5 (ECTS) | ||||||||||||||
| Level of Course | PhD course Ad hoc PhD kursus | ||||||||||||||
| Organisation of Teaching | Section of Environmental Chemistry and Physics, Dept of Plan and Environmental Sciences | ||||||||||||||
| Block Placement | Efter behov | ||||||||||||||
| Language of Instruction | English | ||||||||||||||
| Restrictions | 5 | ||||||||||||||
| Course Content | |||||||||||||||
| A. Theoretical part I. Short overview: Properties, use and occurance of pyrethroids and azoles - use of pyrethroid and azole pesticides - chemical properties: structure, functional groups, stereochemistry, reactivity, stability, . - physicochemical properties: pKa, logKow, bp, . - environmental chemistry (aquatic systems): partitioning between different environmental compartments, half-life in the environment, concentrations measured in the environment,. - environmental toxicology (aquatic systems): biotransformation, bioaccumulation, mode of action, EC50s (TK and TDs),. II. Short overview: Analytical methods used for pyrethroids and azoles mentioned in literature II.1. Chromatography and detection - LC and GC, EI-MS, NCI-MS, ECD, . II.2. Environmental matrices and sample preparation: - water, sediment, aquatic organisms (fish), meat, milk, vegetables, fruits,. - liquid liquid extraction, SPE, SPME, . III. Gas chromatography of azoles and pyrethroids - short introduction into the setup of a GC system: autosampler, injector, GC column - adjustable GC parameters: injection volume, injector temperature, carrier gas flow, temperature ramp, . - different detectors and their sensitivity: EI-MS, NCI-MS, ECD, . - GC methods used in literature   IV. Sample preparation - sample types: see II.2., focus on organisms and water samples - homogenization methods: glas micro mortar, whirl mixer, Potter S, ultrasonic stic, bead mill, . - extraction methods: solvent extraction, liquid liquid extraction (LLE), solid phase extraction (SPE), . - clean up of the extract (removal of H2O, removal of interferences): SPE, Gel permeation chromatography, size exclusion chromatography, . - concentration of analytes: solvent evaporation V. How to develop an analytical method: - choice of solvent, choice of homogenization, extraction and clean up method - choice of suitable GC-ECD parameters - validation of method: determination of matrix effect, recovery, linearity, accuracy, precission,. VI. Analytical method for pyrethroids and azoles in M7 medium and daphnid extracts V.1. Exposure medium (M7): - expected concentration range - liquid liquid extraction with ethylacetate - analysis with GC-ECD V.2. Daphnid samples: - expected internal concentration - homogenization + sample clean up - analysis with GC-ECD VII. Data evaluation - peak integration - quantification of analytes via response ratio  B. Experimental part I. Analytical standards - how to prepare stock solutions of azoles and pyrethroids - how to prepare dilutions - how to prepare standards for calibration curve II. Homogenization of daphnids and clean up of extract - how to use the FastPrep - how to do Solid Phase Extraction - how to concentrate samples III. Liquid liquid extraction - how to shake  - how to dry and concentrate the extract IV. GC-ECD - Intrument check with DFTPP standard - instrument maintenance: changing the liner and septum, cutting the column, . - how to write a method and sequence - how to start a run - test of different GC parameters V. Data evaluation: - peak integration - quantification of analytes   | |||||||||||||||
| Teaching and learning Methods | |||||||||||||||
| The course will consist of kollokier, where relevant litterature is discussed, practical work in the lab, where anayses methods are tested and a final report consisting of a litterature review of the available methods and a critical evaluation of the pro's and con's of the different methods for different purposes. | |||||||||||||||
| Learning Outcome | |||||||||||||||
| The student should be able to analyse pyrethroids and azole pesticides in environmental matrices and to argue for why the specific methods for extraction, cleanup and analyses are used. As analytical tool the focus will be on gas chromatography with electron capture detection (GC-ECD) | |||||||||||||||
| Course Literature | |||||||||||||||
| I. Books: "Synthetic pyretroids". Jay Gan et al. - Chapter 1: Use patterns, properties, and emvironmental effects - Chapter 7: Analytical methology - Chapter 14: Effects of pyrethroids on aquatic organisms - Chapter 18: Chemical analysis and enantioselective toxicity of pyrethroids "Quantitative chemical analysis". Daniel C. Harris "Handbook of residue analytical methods for agrochemicals" - chapters about pyrethroid and azole analysis with GC "Gas chromatography and mass spectrometry: a practical guide". O. David Sparkman And a range of papers (no space in the form for those) | |||||||||||||||
| Course Coordinator | |||||||||||||||
| Nina Cedergreen, ncf@life.ku.dk, Department of Basic Sciences and Environment/Environmental Chemistry and Physics, Phone: 353-33397 Andreas Christopher Kretschmann, ack@life.ku.dk, Department of Basic Sciences and Environment, Phone: 353-32416 | |||||||||||||||
| Course Fee | |||||||||||||||
| None for the sections PhD's | |||||||||||||||
| Type of Evaluation | |||||||||||||||
| The exam is on oral defence of a final report. | |||||||||||||||
| Work Load | |||||||||||||||
| |||||||||||||||