Methods of analysis of chemicals in water, air, biological fluids, tissues, food

A.A. 2020/2021
6
Crediti massimi
48
Ore totali
SSD
CHIM/01 CHIM/06
Lingua
Inglese
Obiettivi formativi
The course will provide theoretical knowledge on the analytical techniques used for the determination of xenobiotics to ensure compliance with relevant obligations and requirements set out by European legislation. Sector specific legislation such as specific rules apply to the EC Clean Air Policy Package or the manufacturing of industrial chemicals, pharmaceuticals, cosmetic products, pesticides, biocides as well as to the control of their residues entering the food production and processing chain and the environment. To exemplify the interdependence between these public health policies and analytical data, emphasis will be placed on the specific legislation:
1. laying down the rules concerning reference methods, data validation and location of sampling points for the assessment of ambient air quality and establishing health based standards and objectives for a number of pollutants present in the air (Directive 2015/1480/EC and Directive 2008/50/EC),
2. establishing specific measures to prevent and control groundwater pollution, setting groundwater threshold values and requiring MS to set their own quality standards applicable to water intended for human consumption (Directive 2006/118/EC and Directive 98/83/EC).
3. Establishing environmental quality standards (EQS) for priority substances and certain other pollutants, with the aim of achieving good surface water chemical status (Directive 2008/105/EC and Directive 2000/60/EC).
4. laying down the rules for authorising sale, use and control of plant protection products in the EU and establishing maximum residue levels of pesticides in or on food and feed of plant and animal origin (Regulation (EC) No 1107/2009, Regulation (EC) No 396/2005, Directive 2002/63/EC ),
5. laying down test methods for the determination of physical-chemical properties (Regulation (EC) No 440/2008) pursuant to the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH regulation), stressing on properties with direct impact on human exposure to chemicals (vapour pressure, water solubility, partition coefficient, acid/base dissociation constant).
Adequate reference will also be given to international conventions and guidelines, as the WHO Guidelines on analytical method validation, the Air Quality Guidelines, the Guidelines for Drinking-Water Quality as well as to the Codex Alimentarius Commission, the Joint FAO/WHO Meeting on Pesticide Residues (JMPR) and the OECD Test Guidelines for Chemicals.
The course will focus on state-of-the-art technologies to be used for the determination of xenobiotics in the environment (soil, water air), in food (plant and animal origin), tissues and body fluids, including sampling (sample collection and sample strategies), sample preparation (the most used extraction techniques for solid and liquid matrices and post-extraction procedures) and analysis: chromatography (GC, LC and IC), mass spectrometry (MS), atomic spectroscopic methods (AAS, ICP-OES, ICP-MS) and XRF. In-field analytical methods as well as continuos monitoring methods will be seen like automated measuring systems as optical particle counters (OPC) for airborne particles. Validation approaches used to ensure accuracy of measurements and compliance with data quality objectives will be addressed.
Students are confronted with measurement uncertainties and common errors committed when preparing samples and working on instruments, the use of significance testing as well as the necessity of method validation.
Students are finally asked to assess exposure and risk of consumers using the calculation model developed by EFSA (PRIMo - Pesticide Residue Intake Model), based on national food consumption figures provided by Member States.
Risultati apprendimento attesi
Educational outcomes/competencies expected are to:
Describe analytical methods commonly used for the determination of urban air pollutants, contaminants in drinking water and residues of active substances in food, tissues and body fluids.
Demonstrate the ability to critically evaluate data obtained for environmental analysis includind all the relevant experimental phases: sampling, sample preparation and analysis.
Demonstrate the ability to critically evaluate data obtained with direct reading monitors.
Demonstrate the ability to critically evaluate data obtained with instruments based on chromatography, spectroscopy and mass spectrometry.
Demonstrate the ability to derive exposure and dose estimates from experimental findings.
Demonstrate an understanding of MRL exceedance/non compliance and ADI/ARfD exceedance.
Demonstrate an understanding of the EU Rapid Alert Systems for food and feed and for non-food chemicals.
Understand physical chemical properties of chemicals and isomers and their role played in human exposure assessment.
Understand the role of method validation and how it is conducted.
Demonstrate knowledge of logarithms, statistical treatment of errors, measuring, weighing and significant figures.
Demonstrate an understanding of the dimensions and units of measurement of physical chemical properties of chemicals.
Demonstrate an understanding of the basic principles of statistical inference and hypothesis testing.
Demonstrate the ability to examine the chemical structure of chemicals with regard to lipo(hydro)philicity, acid/base behaviour, isomerism and readiness to conjugation, detoxification and metabolic breakdown.
Programma e organizzazione didattica

Edizione unica

Responsabile
Periodo
Primo semestre
Attività didattica tradizionale più consultazione dei libri di testo consigliati per una didattica asincrona che integri quella sincrona.
Programma
Il corso fornirà la conoscenza teorica delle tecniche analitiche usate per la determinazione degli xenobiotici. Legislazione settore-specifica quale regole specifiche applicate dalla CE all'impaccamento o la preparazione industriale di prodotti chimici, farmaceutici, pesticidi, biocidi così come pure il controllo dei loro residui che entrano a far parte della produzione e catena di processo ambientale degli alimenti. Enfasi sarà posta sulla legislazione specifica.
Stesura di metodi di valutazione per la determinazione di proprietà chimico-fisiche ai sensi delle norme di Registrazione, Valutazione, Autorizzazione e Restrizione dei prodotti chimici (Regolamento REACH), focalizzando l'attenzione sulle proprietà con impatto diretto sull'esposizione umana alle sostanze chimiche (tensione di vapore, solubilità in acqua, coefficiente di ripartizione, costante di dissociazione acido/base).
Sarà dato adeguato riferimento alle linee guida e convenzioni internazionali.
Il corso si focalizzerà sullo stato dell'arte delle tecnologie usate per la determinazione degli xenobiotici nell'ambiente (suolo, acqua, aria), alimenti (di origine animale o vegetale), tessuti e fluidi biologici, includendo la cromatografia (GC, LC), elettroforesi capillare (CE), plasma accoppiato induttivamente (ICP), tecniche di MS-MS e spettroscopia NMR, mobilità di aerosol e spettrometri di assorbimento ottico differenziale, e approcci di validazione usati per assicurare l'accuratezza delle misure e la conformità con gli obiettivi di qualità.
Gli studenti si confronteranno con l'incertezza delle misure e con i comuni errori commessi quando si preparano i campioni e si lavora sugli strumenti analitici, l'uso del test di significatività e la necessità della validazione del metodo.
Metodi didattici
Slide mostrate a lezione e libri suggeriti
Materiale di riferimento
Materiale del corso: slide presentate a lezione
Libri consigliati:
"Environmental Chemical Analysis" Second Edition S. MItra et al CRC Press (ebook)
"Extraction of Organic Analytes from Foods" A Manual of Methods R. Self The Royal Society of Chemistry (ebook)
"Capillary Electrophoresis-Mass Spectrometry (CE-MS)" Principles and Applications edited by G. De Jong Wiley-VCH (ebook)
"Isotopic Analysis" Fundamentals and Applications using ICP-MS Edited by Frank Vanhaecke and Patrick Degryse Wiley-VCH (ebook)
"Mass Spectrometry" A textbook Third Edition J. Gross Springer (ebook)
"NMR and Chemistry" 4th edition J.W. Akitt, B.E. Mann Taylor & Francis (ebook)
Modalità di verifica dell’apprendimento e criteri di valutazione
L'esame è diviso in una prova scritta (1 ora) seguita da una prova orale. L'esame scritto consiste di 6 domande, tre derivanti dalla parte "Physical-chemical characterization, identity" e tre da "Methods of analysis of chemicals". Gli studenti che superano l'esame scritto saranno ammessi alla prova orale, con domande che riguardano ancora gli argomenti trattati nella prova scritta.
Moduli o unità didattiche
Methods of analysis of chemicals
CHIM/01 - CHIMICA ANALITICA - CFU: 0
CHIM/06 - CHIMICA ORGANICA - CFU: 0
Lectures: 24 ore

Physical-chemical characterization, identity
CHIM/01 - CHIMICA ANALITICA - CFU: 0
CHIM/06 - CHIMICA ORGANICA - CFU: 0
Lectures: 24 ore