55007 - Chemical Toxicological Analysis II

Course Unit Page

SDGs

This teaching activity contributes to the achievement of the Sustainable Development Goals of the UN 2030 Agenda.

Good health and well-being Clean water and sanitation Responsible consumption and production Life on land

Academic Year 2021/2022

Learning outcomes

At the end of the course the student possesses an advanced theoretical and practical knowledge to carry out an updated chemical-toxicological analysis. In particular, the student learns the analytical characteristics of some main pollutants in water, air and soil.
Moreover, the student gains the skills to perform a reliable advanced quali-quantitative analysis, by using the most proper modern techniques and methods applied to biological and non-biological samples.

The course is composed of both lectures and single seat laboratory activities.

Course contents

PROGRAM OF LECTURES:
Module 1 - Analysis of bioactive compounds from biological matrices (Prof. Laura Mercolini)
- Principles, aims and problems of the advanced chemical-toxicological analysis. Peculiar characteristics of advanced chemical-toxicological analysis applied to biologically active compounds in environmental samples and deriving from biological matrices.

- Presentation and description of different specific types of environmental analysis that are necessary due to:

a) Analysis of wastewater for the monitoring of drugs (including doping agents) and metabolites from biological matrices

b) "Wastewater analysis": monitoring of drugs of abuse and metabolites

c) Analysis of soil samples to investigate the presence of hormones from livestock activities.

- Insights and updates on the validation of advanced analytical methods and of the parameters reported in the most recent international guidelines.

- Internal standard (IS) role within advanced environmental quantitative analysis.

- Advanced methods for sample collection and pretreatment: simplified liquid extraction (SLE), disposable pipette tip extraction (DPX), stop and go extraction tips (StAGE), microextraction on packed sorbent (MEPS), disposable microfibers for solid phase microextraction (SPME).

- Capillary electrophoresis (CE): physicochemical principles and applications to the environmental analysis.

- UHPLC for the environmental analysis: general principles and applications.

- Electrochemical detection based on the use of amperometric and coulometric detectors.

- High resolution mass spectrometry (HRMS): applications to the most significant and recent issues of advanced environmental analysis.


PROGRAM OF LECTURES:
Module 2 - Analysis of environmental pollutants from anthropogenic activities (Dr. Michele Protti)
- Presentation and description of different specific types of environmental analysis applied to pollutants from entropic activity that are necessary due to:

a) Exposure to active ingredients (API) in the workplace, analytical assessment of the effectiveness of containment strategies

b) Analysis of water (river or wastewater) for monitoring endocrine disrupting chemicals (EDC) from industrial production

c) Soil analysis of EDC from industrial production.

- Quality control of products containing biologically active molecules of interest for the purpose of monitoring environmental matrices.

- Advanced methods for sample collection and pretreatment: extraction by nylon filtration, vortex-assisted liquid-liquid micro extraction (VALLME), dispersive liquid-liquid microextraction (DLLME), dispersive sample pretreatment (DSP).

- IR spectroscopy: advanced analysis principles and applications.


PROGRAM OF THE LABORATORY ACTIVITIES
Module 1 - Analysis of bioactive compounds from biological matrices (Prof. Laura Mercolini)
1) MEPS-HPLC-PDA analysis of clozapine and N-desmethylclozapine in wastewater
2) DPX-HPLC-PDA analysis of clenbuterol in wastewater
3) SLE-HPLC-PDA analysis of steroids in soil.

 

PROGRAM OF THE LABORATORY ACTIVITIES
Module 2 - Analysis of environmental pollutants from anthropogenic activities (Dr. Michele Protti)
1) Qualitative analysis of antibiotics in samplers for the control of airborne particulate by TLC and IR spectroscopy
2) Quantitative analysis of antibiotics in samplers for the control of airborne particulate by UV spectrophotometry
3) HPLC-PDA analysis of bisphenol A in river water by nylon filtration extraction
4) HPLC-PDA analysis of nonylphenol in wastewater by VALLME
5) SPE-HPLC-PDA analysis of clozapine in industrial wastewater
6) Quality control of clenbuterol in a pharmaceutical formulation and a prohibited product.


 

 

 

Readings/Bibliography

STUDY MATERIALS:
- Slides presented and discussed during the lectures
- Papers from the scientific literature
- Videos and similar materials
- Handout of the laboratory experiments.


FURTHER MATERIALS:

- Carrieri A. "Manuale di Analisi Quantitativa dei Medicinali"
EDISES, Napoli, 2019.
- Holler J.F., Crouch S.R. “Fondamenti di Chimica Analitica” di Skoog & West, EdiSES s.r.l., 2015.
- Hage D.S., Carr J.D. "Chimica Analitica e Analisi Quantitativa", Piccin, 2012.
- Skoog D.A., Holler J.F., Crouch S.R., Sabbatini L. “Chimica Analitica Strumentale”, EdiSES s.r.l., 2009.
- Ana Isabel Morales Martin et al. "Challenges in Open Educational Resources: the case of TOX-OER MOOC"
Editore Amarante; first edition 2018.

 

 

 

Teaching methods

Considering the activities and teaching methods adopted in this course, attending it requires the students to have already completed modules 1 and 2 (in e-learning mode at this web address, as well as module 3 (in person) of the specific "Health and Safety in places of study" course. An updated schedule and the manner of attending module 3 are available in the corresponding section of the Graduation Programme webpage.

The course consists of lectures (32 h, 4CFU) during which the main instrumental techniques and methods required for the advanced environmental analysis are discussed.
The course deals also with single seat laboratory activities (36 h, 3 CFU), during which the student prepares a laboratory notebook. The laboratory activities offer the student the opportunity of carrying out different types of advanced analysis for identification and quantitation of the compounds of interest in environmental matrices, by firsthand using the techniques and methodologies required to perform such analyses.


The course consists of exactly two modules:
Module 1 - ANALYSIS OF BIOACTIVE COMPOUNDS FROM BIOLOGICAL MATRICES - 4 CFU, of which 3 CFU (24 hours) of theoretical lectures and 1 CFU (12 hours) of laboratory activities - Prof. Laura Mercolini.

Module 2 - ANALYSIS OF ENVIRONMENTAL POLLUTANTS FROM ANTHROPOGENIC ACTIVITIES - 3 CFU, of which 1 CFU (8 hours) of theoretical lectures and 2 CFU (24 hours) of laboratory activities - Dr. Michele Protti.



Lecture attendance is very important for a satisfactory learning process.
Laboratory activity attendance is mandatory for the learning process.
The student can take the oral exam for the modules in the same day and anyway within the same session, and finally will get one overall grade for the course of Chemical Toxicological Analysis II.

 

Assessment methods

The learning assessment aims at verify practical skills and theoretical knowledge acquired by the student while attending both the lectures and the laboratory experiences. In particular the following skills will be evaluated:

- Mastery of the advanced instrumental analytical terminology and of the theoretical basis of the discussed topics;

- Ability to perform laboratory procedures for the quali-quantitative analysis;

- Specific training on the uses, reactions, toxicity and analytical procedures of the examined compounds;

- Critical processing and evaluation of the laboratory analytical results.

The assessment of the learning is performed on the basis of an oral examination consisting of some questions (5 to 10 questions) about both the theoretical and the practical parts.
The student could also be asked to comment on a paper from the scientific literature and chosen among those presented and discussed during the lectures, with the possibility for the student to consult the paper itself.
Moreover, during the laboratory activities for each module, it is planned to carry out practical tests the results of which are reported by the student within his/her own laboratory notebook, evaluated by the teacher, and which is part of the final score. For each module the student must prepare the laboratory notebook.
The file of the laboratory notebook has to be sent by mail to the teacher of the relate module at least one week before taking the oral exam.

 

 

Teaching tools

Lectures are carried out by means of the common electronic media, such as pc, tablet, smartphone and similar devices connected to a videoprojector and to the wi-fi.
Within module 1, the 3-hour e-learning lecture is carried out by using a MOOC (Massive Online Open Courses) approach on TOX-OER Moodle.

The practical activities are developed in specially equipped didactic laboratories where each student has at disposal a single place of work, all the instrumentations and materials necessary to perform an advanced chemical-toxicological environmental analysis.

Office hours

See the website of Laura Mercolini

See the website of Michele Protti