ANALISI DEI FARMACI E DEI PRODOTTI PER LA SALUTE 3 M - Z

Academic Year 2025/2026 - Teacher: ANGELO SPADARO

Expected Learning Outcomes

Knowledge and understanding: the student must acquire the theoretical and practical preparation for the recognition of organic compounds of pharmaceutical interest reported in the monographs of the official pharmacopoeias, through instrumental analytical techniques and chemical tests. 
The student must also acquire the theoretical basis of the main analytical techniques for the analysis of active ingredients in biological matrices.

Application of knowledge and understanding. The student must be able to use the knowledge acquired in the field of pharmaceutical analysis to develop and validate analysis protocols on active ingredients in pharmaceutical forms and biological matrices.

Autonomy of judgment. The student must be able to interpret the experimental results obtained relating to the analysis of active ingredients present in pharmaceutical forms and complex matrices.

Communication skills. At the end of the course the student must be able to present what has been learned using an appropriate terminology for a correct scientific presentation regarding the analytical techniques and the analysis of compounds of pharmaceutical interest.

Learning skillsThe student will have developed theoretical and practical skills to update and expand their knowledge, enabling them to address new analytical challenges.

Course Structure

Frontal lessons (28 hours) and laboratory exercises (30 hours).

If the teaching is taught in mixed or distance mode, the necessary changes may be introduced with respect to what was previously declared, in order to respect the planned program and reported in the syllabus..

Required Prerequisites

The basic knowledge required for a profitable and easy access to the course concerns General and Inorganic Chemistry, Organic Chemistry (propaedeutic), Physics, Analysis of Drugs and Health Products 1 and 2.

Attendance of Lessons

Mandatory.

Detailed Course Content

Introduction to instrumental analytical methods. Classification of instrumental analytical methods. Choice of analytical method. Ultraviolet and visible absorption and emission spectroscopy (fluorescence and phosphorescence). Infrared absorption spectroscopy. Mass spectrometry. Nuclear magnetic resonance spectrometry (1H- and 13C-NMR).

Chemical tests for recognition of organic functional groups. Determination of chemical-physical constants.

Chromatographic techniques and applications. General principles of the chromatographic process and chromatographic parameters: distribution constant, retention time. capacity factor. Resolution. Selectivity. Efficiency: plate theory; van Deemter equation. Chromatographic peak asymmetry.

Liquid chromatography: stationary phase, mobile phase. Liquid-solid chromatography, liquid-liquid chromatography, ion exchange chromatography, ion pair chromatography, size exclusion chromatography, affinity chromatography. Column chromatography, thin layer chromatography (TLC). High performance liquid chromatography (HPLC): instrumentation. Enatioselective chromatographic separation: direct method using enantioselective stationary phases.

Gas chromatography (GC): instrumental aspects, types of stationary phase, GC detection. Capillary electrophoresis (CE): instrumentation, theoretical principles, analytical parameters.

Mass spectrometry and applications: classes of instrumentation, ionization techniques, fragmentation analysis, analyzers and detector. Combined techniques: liquid chromatography and UV-VIS photodiode detector (HPLC-DAD), liquid chromatography and mass spectrometry (HPLC-MS), gas chromatography and mass spectrometry (GC-MS).

Qualitative and quantitative analysis (external standard method, internal standard method). Sample preparation and extraction methods. Classical extraction methods (liquid/liquid and liquid/solid). Supercritical fluid extraction (SFE). Solid phase extraction (SPE). Sample preparation from complex biological matrices.

Analytical method validation: linearity, precision, accuracy, reproducibility, limit of detection (LOD), limit of quantification (LOQ). Development of chromatographic methods for quality control and in pre-clinical and clinical research. Determination of drug/target protein interactions, by high-performance affinity chromatography (HPAC), for the development of new drugs.

Course Planning

 SubjectsText References
1Introduction to instrumental analytical methods. Classification of instrumental analytical methods. Choice of analytical method. Ultraviolet and visible absorption and emission spectroscopy (fluorescence and phosphorescence). Infrared absorption spectroscopy. Mass spectrometry. Nuclear magnetic resonance spectrometry (1H- and 13C-NMR).1-4 and teaching material
2Chemical tests for recognition of organic functional groups. Determination of chemical-physical constants.1-3 and teaching material
3Chromatographic techniques and applications. General principles of the chromatographic process and chromatographic parameters: distribution constant, retention time. capacity factor. Resolution. Selectivity. Efficiency: plate theory; van Deemter equation. Chromatographic peak asymmetry.2-4 and teaching material
4Liquid chromatography: stationary phase, mobile phase. Liquid-solid chromatography, liquid-liquid chromatography, ion exchange chromatography, ion pair chromatography, size exclusion chromatography, affinity chromatography. Column chromatography, thin layer chromatography (TLC). High performance liquid chromatography (HPLC): instrumentation. Enantioselective chromatographic separation: direct method using enantioselective stationary phases. Gas chromatography (GC): instrumental aspects, types of stationary phase, GC detection. Capillary electrophoresis (CE): instrumentation, theoretical principles, analytical parameters.2-4 and teaching material
5Spettrometria di Massa e applicazioni: classi di strumentazioni, tecniche di ionizzazione, analisi della frammentazione, Analizzatori e rilevatore. Tecniche combinate: cromatografia liquida e rivelatore UV-VIS a fotodiodi (HPLC-DAD), cromatografia liquida e spettrometria di massa (HPLC-MS), gascromatografia e spettrometria di massa (GC-MS).1-4 and teaching material
6Qualitative and quantitative analysis (external standard method, internal standard method). Sample preparation and extraction methods. Classical extraction methods (liquid/liquid and liquid/solid). Supercritical fluid extraction (SFE). Solid phase extraction (SPE). Sample preparation from complex biological matrices.2-4 and teaching material
7Analytical method validation: linearity, precision, accuracy, reproducibility, limit of detection (LOD), limit of quantification (LOQ). Development of chromatographic methods for quality control and in pre-clinical and clinical research. Determination of target drug/protein interactions, by high-performance affinity chromatography, for the development of new drugs.2-4 and teaching material

Learning Assessment

Learning Assessment Procedures

The evaluation of learning will be conducted through a written and/or oral exam.

The evaluation may also be conducted online, should the conditions require it.

The exam schedule is published on the Department of Pharmaceutical and Health Sciences website (www.dsf.unict.it).

Examples of frequently asked questions and / or exercises

Theoretical principles of chromatographic separations: approaches to improve resolution in liquid chromatography. Theoretical principles and applications of capillary electrophoresis. Sample preparation and extraction methods. Validation of the analytical method. Chemical recognition of amines of pharmaceutical interest. Describe the apparatus scheme of the mass spectrometer.