OVERVIEW

The course presents the theoretical knowledge of the main analytical instrumental methods used in the qualitative and quantitative analysis of substances for medicinal use, pure or in pharmaceutical preparations, and briefly describes the instrumentation and the related mechanism of operation. Finally the laboratory exercises (individual or group) allow the practical application of the theoretical concepts treated.

AIMS AND CONTENT

LEARNING OUTCOMES

The course consists of a theoretical part and a practical section (laboratory exercises). It aims to provide basic knowledge on the main instrumental analytical methods used in the quali-quantitative analysis of medicinal substances, pure or contained in pharmaceutical preparations. Knowledge on theoretical principles, applications in the pharmaceutical analysis and essential technical aspects of the instrumentation are provided in addition to theoretical and practical knowledge of modern methods of extraction from complex matrices.

AIMS AND LEARNING OUTCOMES

The course aims to provide basic knowledge of analytical spectroscopic (Uv_Vis), chromatographic (HPLC and GC) and electrophoretic analytical methods for qualitative and quantitative applications. At the end of the theoretical and practical lessons the student is able to

- Know the theories underlying instrumental analytical methods

- Evaluate the applicability of the analytical methods

- Use spectrophotometric and chromatographic instrumentation through laboratory exercises

- Apply analytical sample pretreatment methods

- Present data and results of exercises carried out through reports sent via website “AulaWeb”.

PREREQUISITES

Knowledge of inorganic and organic analysis with classical methods is required, as well as knowledge of organic chemistry to understand the physico-chemical properties of drugs (acidity / basicity, hydrophilicity / lipophilicity, types of chemical interaction).

TEACHING METHODS

The course takes place through lectures and laboratory exercises (individual and group). At the end of each exercise, the student must provide a report containing data, calculations and results of the exercise. The teaching material is provided on the AULAWEB online site.

In consideration of the current health situation, the theoretical lessons can be delivered online. The laboratory exercises may be reduced and/or replaced by "alternative" teaching.

SYLLABUS/CONTENT

Introduction and classification of instrumental analytical methods

Analytical instrumentation: signal units; detectors; signal integrators and computers.

Significant figures: precision, sensitivity, accuracy, limit of detection and quantitation, selectivity.Signal and noise.

Spectroscopy

Electromagnetic radiation. Interaction with matter: absorption and amission. Lambert-Beer’s law.

Instrumentation: radiation sources, wavelength selectors, detectors.

Visible-ultraviolet molecular spectroscopy. Qualitative and quantitative applications.

Fluorescence and phosphorescence. Characteristcs of methods. Qualitative and quantitative applications. Derivatization methods.

Atomic absorption and emission spectroscopy. Atomizers. Flame atomization, plasma emission. Pharmaceutical applications.

Chromatography

Classification of chromatographical methods. Theory of separation processes: Van Deemter’s equation. Efficiency and resolution.

Gas chromatography. General basics. Instrumentation. Hyphenated techniques. Qualitative and quantitative applications. Derivatization methods.

High-performence liquid chromatography. General basics. Stationary and mobile phases. Instrumentation. Qualitative and quantitative applications. Derivatization methods.

Ion chromatography and size-exclusion chromatography.

Capillary electrophoresis

General basics. Instrumentation, Pharmaceutical applications.

Sample preparation

Supercritical fluid extraction: general basics, instrumentation, applications.

Solid-phase extraction: general basics, instrumentation and material, applications.

Chiral drugs analysis. Enantiomeric mixtures. Chiral chromatographical methods. Chiral Phases.

RECOMMENDED READING/BIBLIOGRAPHY

- Chimica Analitica Strumentale - Holler, Skoog, Crouch.- EdiSES 2009

- Fondamenti di chimica analitica – Skoog, West – EdiSES 2015

- Analisi farmaceutica - D. G. Watson - Edra 2014

TEACHERS AND EXAM BOARD

Exam Board

BRUNO TASSO (President)

ANDREA SPALLAROSSA

CHIARA BRULLO (Substitute)

LESSONS

Class schedule

The timetable for this course is available here: Portale EasyAcademy

EXAMS

EXAM DESCRIPTION

Oral examination (about 40 minutes, 3-4 questions). For the final evaluation the result of the laboratory exercises is also taken into account (divided into three merit ranges).

ASSESSMENT METHODS

In laboratory exercises the student must demonstrate the correct and adeguate manual skills. In the preparation of reports should demonstrate the ability of setting the correct calculation and clear presentation of results. During the oral exam, students must demonstrate theoretical knowledge of analytical techniques and reasoning skills to solve analytical problems by comparison of analytical techniques.

Exam schedule