55006 - Chemical Toxicological Analysis I

Learning outcomes

The course aim to give the theoretical and practical knowledge to design and execute chemical toxicological analyses.

At the end of the course the student is supposed to know the main spectroscopic and separative techniques and methods for environmental analysis. he should also be able to read and understand approved protocols and to apply the suitable analytical technique to solve a specific analytical problem.

Course contents

"BASIC PRINCIPLES" (1 + 1 credits )  

Prof. Carlo Bertucci

Aims and problems of chemical-toxicological analysis. Introduction to protocols for environmental analysis from regulatory authorities. Analytical method validation: validation parameters. Working scales, analyte concentration and their influence on the choice of the analytical technique. Sampling methods. Sample pre-treatment: liquid-liquid extraction, solid-liquid extraction and solid phase extraction and microextraction.

"SPECTROSCOPIC AND SEPARATIVE TECHNIQUES" (3 + 3 credits)

Dr. Manuela Bartolini

Polarimetry: chirality and optical rotation, enantiomeric excess, biological significance of chirality, polarimetric analysis.

Refractometry. Definition of refractive index. Abbe refractometer.

Atomic absorption spectroscopy (AA) and emission spectroscopy: Principles of the techniques. Instrumentation. Application to the environmental analysis.

IR spectroscopy: theory and instrumentation. Identification and quantitation of the analytes.

UV-vis spectroscopy. Theory and relationship between UV absorption and chemical structure. Absorbance and trasmittance; Experimental determination of the molar extinction coefficient. Quantitative analysis: Lambert Beer law, calibration curve construction, wavelength selection for quantitative analysis, selectivity. Deviations from the Lambert Beer Law. Derivative spectrophotometry: analysis of binary mixture. Differential spectroscopy. Multi-component analysis. Applications to chemical toxicological analysis. Characteristics and limitations of this technique.

 Fluorometry Excitation and emission spectra. Quenching phenomena. Quali-quantitative analyses of pollulants. Chemical fluorescence derivatisation.

Mass spectrometry: theoretical basis. Ion sources and mass analyzers (single quadrupole, triple quadrupole, ion trap, time-of-fly). Ionisation techniques.  Acquisition modes.  Applications.

Spettrometria di massa: basi teoriche, descrizione delle componenti dello strumento. Tecniche di ionizzazione. Tipologie di sorgenti e di analizzatori di massa. Vantaggi e svantaggi della tecnica. Applicazioni generali e specifiche all'analisi ambientale.

Chromatographic techniques in drug analysis General concepts and principal classification of chromatographic techniques: liquid chromatography and gas chromatography. Instrumentation and available detectors. Theory of chromatographic separations: retention time, efficiency, selectivity, capacity factor, resolution. Van Deemter equation. Applications to the environmental analysis.

Readings/Bibliography

V. Cavrini, V. Andrisano. ANALISI FARMACEUTICA: Metodi di Riconoscimento e di Separazione. Seconda Edizione (2009) Società Editrice Esculapio

EPA methods (www.epa.gov) for environmental analyses

APAT-IRSA-CNR protocols for water

Presented slides and scientific literature discussed during the course

Teaching methods

The corse is divided in two parts: "Basic Principles" and "spectroscopic and separative techniques".

"Basic principles" consists of both lectures (8 h teaching) and laboratory activities (12 h).
"Spectroscopic and separative techniques" consists of both lectures (24 h teaching) and laboratory activities (36 h).

The student is supposed to fill up a laboratory folder containing all the experiences carried out during laboratory activities.

Assessment methods

Oral discussion on the course content and discussion on practical experiences carried out during the course. Personal laboratory folder must be clearly written and is part of the final evaluation.

Office hours

See the website of Manuela Bartolini

See the website of Carlo Bertucci