Methods of Analysis of Chemicals in Water, Air, Biological Fluids, Tissues, Food

A.Y. 2024/2025
6
Max ECTS
48
Overall hours
SSD
CHIM/01 CHIM/06
Language
English
Learning objectives
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.
Expected learning outcomes
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.
Single course

This course can be attended as a single course.

Course syllabus and organization

Single session

Responsible
Lesson period
First semester
Course syllabus
The course will provide theoretical knowledge on the analytical techniques used for the determination of xenobiotics. Sector specific legislation such as specific rules apply to the EC Clean Air Policy Package or the manufacturing of industrial chemicals, pharmaceuticals, pesticides, biocides as well as to the control of their residues entering the food production and processing chain and the environment. Emphasis will be placed on the specific legislation.
Laying down test methods for the determination of physical-chemical properties 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.
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 chromatography (GC, LC ), capillary electrophoresis (CE), inductively coupled plasma (ICP), hyphenated MS-MS techiques and NMR spectroscopy, aerosol mobility and differential optical absorption spectrometers, as well as the validation approaches used to ensure accuracy of measurements and compliance with data quality objectives.
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.
Teaching methods
Lessons slides and suggested books
Teaching Resources
Course material: lesson slides.
Books suggested:
"Capillary Electrophoresis-Mass Spectrometry-Applications"-De Jong (ebook)
"Isotopic Analysis-Fundamentals and Applications using ICP-MS"-Patrick Degryse (ebook)
"Mass Spectrometry-A Textbook" J. H. Gross (ebook)
"NMR-From Spectra to Sructures An Experimental Approach"-T.N. Mitchell B. Costisella (ebook)
Assessment methods and Criteria
The examination is devided into a written exam (1 hour) followed by the oral examination. The written exam consists on 6 questions, three derived from "Physical-chemical characterization, identity" and three from "Methods of analysis of chemicals". Students that pass the written exam will be allowed to discuss the oral exam, with questions still embracing the arguments addressed in the written exam.
Methods of analysis of chemicals
CHIM/01 - ANALYTICAL CHEMISTRY - University credits: 3
Lectures: 24 hours
Professor: Schlitt Christian
Physical-chemical characterization, identity
CHIM/06 - ORGANIC CHEMISTRY - University credits: 3
Lectures: 24 hours
Professor: Fedrizzi Giorgio