Methods of analysis of chemicals in water, air, biological fluids, tissues, food
A.A. 2018/2019
Learning objectives
The course will provide theoretical and practical knowledge on the qualitative and quantitative techniques for the identification and characterization of xenobiotics in different matrices (food, air, water, etc. ..) on the basis of the request of REACH and other relevant European regulations. Methods to monitor xenobiotics in the environment and in living organisms include measurements of environmental and tissue concentrations of contaminants: both external (air, water, food, and soil) and internal (blood, urine, breast milk, adipose tissue, and muscle tissue): the course will focus on state-of-the-art technologies to be used for such analyses including gas and liquid chromatography, high performance liquid chromatography, mass spectrometry, and high-resolution mass spectrometry (HRMS). Emphasis will be given to the OECD/EU regulations for the use of these technologies in the xenobiotics measurement.
Expected learning outcomes
Non definiti
Periodo: Primo semestre
Modalità di valutazione: Esame
Giudizio di valutazione: voto verbalizzato in trentesimi
Corso singolo
Questo insegnamento non può essere seguito come corso singolo. Puoi trovare gli insegnamenti disponibili consultando il catalogo corsi singoli.
Course syllabus and organization
Edizione unica
Responsabile
Periodo
Primo semestre
Prerequisiti
The examination of "Methods of analysis of chemicals in water, air, biological fluids, tissues, food" is made up of two parts: one written exam with 6 questions, three derived from "Physical-chemical characterization, identity" and three from "Methods of analysis of chemicals".
The students that pass the written exam will be able to sustain the oral exam, with questions about both parts of the Course during the same session.
The students that pass the written exam will be able to sustain the oral exam, with questions about both parts of the Course during the same session.
Methods of analysis of chemicals
Programma
Introduction to REACH Regulation (2 hours)
1. Aim of REACH;
2. Supply chain, actors, roles;
3. Registration timeline;
4. Evaluation, Authorisation and Restriction.
Introduction to PPPR Regulation (2 hours)
1. Directives 79/117/EEC to 91/414/EEC;
2. Regulation (EC) No 1107/2009;
3. Regulation (EC) No 396/2005.
Physical-chemical characterization of chemicals (I) (4 hours)
1. Section 1 data requirements: Melting, boiling point and temperature of decomposition, Vapour pressure and Henry's law constant, Solubility in water and in organic solvents, Surface tension, Partition coefficient, Dissociation constant, UV/VIS absorption, Flammability, Flash point, Explosive and Oxidising properties;
2. Geometric and Optical Isomers;
3. CLP-Regulation (EC) 1272/2008.
Measurement Uncertainty (I) (2 hours)
1. Accuracy; Precision, Repeatability, Reproducibility;
2. Gross error, Dixon's Q;
3. Gaseous, liquid and solid samples;
4. Glassware and weights;
5. Sample preparation and instrumental analysis.
Dietary Exposure Assessment to Pesticide Residues (I) (4 hours)
1. Setting of MRLs;
2. GAP; STMR; TMDI, NEDI; NESTI;
3. Supervised field trials and livestock feeding studies;
4. EFSA PRIMO model;
5. EU-coordinated Multi-Annual Pesticide Control Program;
6. Directive 2002/63/EC and FAO CAC/GL 33-1999;
7. RASFF.
Measurement Uncertainty (II) (4 hours)
1. Storage stability;
2. Purification & extraction efficiency;
3. Radiolabelling;
4. Calibration and blanks;
5. GC & LC amenability and troubleshooting;
6. Detection, quantitation & confirmation;
7. Significance testing and propagation of errors.
Method validation (I): Parameters and Guidelines (4 hours)
1. Specificity, Linearity, Accuracy, Precision, LOQ, Robustness;
2. Active substance and impurities in TK/TC and PPP (SANCO/3030/99);
3. RA methods: residues in foodstuff, soil, water and air (SANCO/3029/99);
4. MON/ENF methods: residues in foodstuff, soil, water, air and body fluids (SANCO/825/00);
5. Official controls (SANCO/12571/2013);
6. QuEChERS, QuPPe and Single Residue Methods (SRM).
Physical-chemical characterization of chemicals (II) (2 hours)
1. Manufacturing process and specification;
2. Vapour pressure and flash point;
3. Lipophilicity, logP;
4. Dissociation and hydrolysis;
5. RAPEX.
Method validation (II): (2 hours)
Real world applications - EXERCISES
1. Determination of impurities in technical material
2. Determination of residues in plant material
3. Determination of residues in body fluids
Dietary Exposure Assessment to Pesticide Residues (II) (2 hours)
Real world applications - EXERCISES
4. Nature of metabolites (TRR)
5. Supervised residue trial on mais
6. Running EFSA Primo Model
1. Aim of REACH;
2. Supply chain, actors, roles;
3. Registration timeline;
4. Evaluation, Authorisation and Restriction.
Introduction to PPPR Regulation (2 hours)
1. Directives 79/117/EEC to 91/414/EEC;
2. Regulation (EC) No 1107/2009;
3. Regulation (EC) No 396/2005.
Physical-chemical characterization of chemicals (I) (4 hours)
1. Section 1 data requirements: Melting, boiling point and temperature of decomposition, Vapour pressure and Henry's law constant, Solubility in water and in organic solvents, Surface tension, Partition coefficient, Dissociation constant, UV/VIS absorption, Flammability, Flash point, Explosive and Oxidising properties;
2. Geometric and Optical Isomers;
3. CLP-Regulation (EC) 1272/2008.
Measurement Uncertainty (I) (2 hours)
1. Accuracy; Precision, Repeatability, Reproducibility;
2. Gross error, Dixon's Q;
3. Gaseous, liquid and solid samples;
4. Glassware and weights;
5. Sample preparation and instrumental analysis.
Dietary Exposure Assessment to Pesticide Residues (I) (4 hours)
1. Setting of MRLs;
2. GAP; STMR; TMDI, NEDI; NESTI;
3. Supervised field trials and livestock feeding studies;
4. EFSA PRIMO model;
5. EU-coordinated Multi-Annual Pesticide Control Program;
6. Directive 2002/63/EC and FAO CAC/GL 33-1999;
7. RASFF.
Measurement Uncertainty (II) (4 hours)
1. Storage stability;
2. Purification & extraction efficiency;
3. Radiolabelling;
4. Calibration and blanks;
5. GC & LC amenability and troubleshooting;
6. Detection, quantitation & confirmation;
7. Significance testing and propagation of errors.
Method validation (I): Parameters and Guidelines (4 hours)
1. Specificity, Linearity, Accuracy, Precision, LOQ, Robustness;
2. Active substance and impurities in TK/TC and PPP (SANCO/3030/99);
3. RA methods: residues in foodstuff, soil, water and air (SANCO/3029/99);
4. MON/ENF methods: residues in foodstuff, soil, water, air and body fluids (SANCO/825/00);
5. Official controls (SANCO/12571/2013);
6. QuEChERS, QuPPe and Single Residue Methods (SRM).
Physical-chemical characterization of chemicals (II) (2 hours)
1. Manufacturing process and specification;
2. Vapour pressure and flash point;
3. Lipophilicity, logP;
4. Dissociation and hydrolysis;
5. RAPEX.
Method validation (II): (2 hours)
Real world applications - EXERCISES
1. Determination of impurities in technical material
2. Determination of residues in plant material
3. Determination of residues in body fluids
Dietary Exposure Assessment to Pesticide Residues (II) (2 hours)
Real world applications - EXERCISES
4. Nature of metabolites (TRR)
5. Supervised residue trial on mais
6. Running EFSA Primo Model
Physical-chemical characterization, identity
Programma
Introduction to physical and chemical characteristics of xenobiotics (Log P, Log D, lipophilicity) 1 hour
1. Physical and chemical parameters to be considered
Introduction to Matrices Extraction 4 hours
1. The importance of sampling to achieve the extraction from complex matrices
2. Physical-chemical properties of drugs and their extraction from biological material
3. Sample pretreatment in different biological matrices
4. Methods of extraction: SPE, SPME, SFE, MSPD
Capillary Electrophoresis And Drug Analysis 4 hours
1. Introduction to Capillary electrophoresis as a powerful separation technique which proved sufficiently competitive /complementary to high performance liquid chromatography (HPLC)
2. Modes of separation, EOF, analytes' physicalchemical characteristics and techniques used
3. CE different techniques: CZE, CGE, EKC, ITP, MEKC
4. CE applications in xenobiotics analysis
Inductively Coupled Plasma (ICP) 4 hours
1. Introduction to ICP techniques: theory
2. ICP-EOS (Optical Emission Spectroscopy)
3. ICP-MS (Mass Spectrometry)
4. Xenobiotics analysis: possible applications
Introduction to NMR Technique and Drug Analysis 12 hours
1. Introduction to NMR Xenobiotics analysis
2. Proton and Carbon NMR Spectroscopy
3. Chemical shift, spin-spin coupling: n+1 rule, second order spectra, solvent effects, relaxation processes
4. NMR experiments as powerful technique in drug analysis: pulse, acquisition time, magnetization, FID, FT
5. NMR applications: 1H NMR, 13C NMR
6. NMR exercises to recognize organic molecules in biological fluids.
1. Physical and chemical parameters to be considered
Introduction to Matrices Extraction 4 hours
1. The importance of sampling to achieve the extraction from complex matrices
2. Physical-chemical properties of drugs and their extraction from biological material
3. Sample pretreatment in different biological matrices
4. Methods of extraction: SPE, SPME, SFE, MSPD
Capillary Electrophoresis And Drug Analysis 4 hours
1. Introduction to Capillary electrophoresis as a powerful separation technique which proved sufficiently competitive /complementary to high performance liquid chromatography (HPLC)
2. Modes of separation, EOF, analytes' physicalchemical characteristics and techniques used
3. CE different techniques: CZE, CGE, EKC, ITP, MEKC
4. CE applications in xenobiotics analysis
Inductively Coupled Plasma (ICP) 4 hours
1. Introduction to ICP techniques: theory
2. ICP-EOS (Optical Emission Spectroscopy)
3. ICP-MS (Mass Spectrometry)
4. Xenobiotics analysis: possible applications
Introduction to NMR Technique and Drug Analysis 12 hours
1. Introduction to NMR Xenobiotics analysis
2. Proton and Carbon NMR Spectroscopy
3. Chemical shift, spin-spin coupling: n+1 rule, second order spectra, solvent effects, relaxation processes
4. NMR experiments as powerful technique in drug analysis: pulse, acquisition time, magnetization, FID, FT
5. NMR applications: 1H NMR, 13C NMR
6. NMR exercises to recognize organic molecules in biological fluids.
Moduli o unità didattiche
Methods of analysis of chemicals
CHIM/01 - CHIMICA ANALITICA
CHIM/06 - CHIMICA ORGANICA
CHIM/06 - CHIMICA ORGANICA
Lectures: 24 ore
Docente:
Schlitt Christian
Physical-chemical characterization, identity
CHIM/01 - CHIMICA ANALITICA
CHIM/06 - CHIMICA ORGANICA
CHIM/06 - CHIMICA ORGANICA
Lectures: 24 ore
Docente:
Fedrizzi Giorgio
Professor(s)