ANALISI FARMACEUTICA E NUTRACEUTICO-ALIMENTARE 2 M - Z

Knowledge and understanding. The student will have to acquire the theoretical and practical skills useful for the recognition of organic compounds of pharmaceutical interest reported in the monographs of official pharmacopoeias, through specific chemical assay and instrumental analytical techniques. The student will also acquire the theoretical bases of the main analytical techniques for the analysis of active principles in biological matrices.

Applying knowledge and understanding. The student must be able to use the knowledge acquired in the context of instrumental analysis to develop and validate analysis protocols for the analysis of active ingredients in pharmaceutical forms and biological matrices.

Making judgments: The student will have to interpret the experimental results obtained relating to the analysis of active ingredients present in complex matrices.

Communication skills: At the end of the course the student will have to explain what has learned using appropriate terminology for a correct scientific presentation regarding the analytical techniques and the analysis of compounds of pharmaceutical interest.

Learning skills. The student will have to developed useful theoretical/practical skills in order to update and expand his knowledge with the aim of face new analytical problems.

Frontal lessons (42 hrs) and laboratory training (45 hrs).

Should teaching be carried out in mixed mode or remotely, it may be necessary to introduce changes with respect to previous statements, in line with the programme planned and outlined in the syllabus.

Information for students with disabilities and / or SLD: To guarantee equal opportunities and in compliance with the laws in force, interested students can ask for a personal interview in order to plan any compensatory and / or dispensatory measures, based on the teaching objectives and specifications needs. It is also possible to contact the CInAP contact person (Center for Active and Participatory Integration - Services for Disabilities and / or SLD) of the DEPARTMENT OF DRUG AND HEALTH SCIENCES, Prof. Teresa Musumeci.

Attendance in the classroom is mandatory. The maximum limit of absences allowed is 30% as reported in the teaching regulations of the CdS which can be consulted on the website of the Department of Pharmaceutical and Health Sciences. Once this limit has been exceeded, it will not be possible to access the practical laboratory exercises.

LECTURES 

Identification of compounds registered in the FUI and Pharm. Eur. Preliminary assays: organoleptic characters and combustion behaviour of substances. Solubility in water and reactive solvents; classification of substances according to their solubility. 

Functional groups and assays for recognition: carboxylic acids and derivatives, hydroxy acids, phenols, alcohols, aldehydes and ketones, halogen derivatives, amines, and nitro compounds. Recognition of carbohydrates and amino acids.

Determination of physical constants: melting point, boiling point, refractive index, rotational optical power. CHNO Elemental Analyzer - sample preparation and qualitative-quantitative analysis.

Chromatographic techniques. General principles of the chromatographic process and chromatographic parameters. Distribution constant. Retention time. Capacity factor. Selectivity. Efficiency: plate theory; van Deemter equation; extra-column effects.  Chromatographic peak asymmetry. Resolution.

Liquid chromatography: stationary phase, mobile phase. Liquid-solid chromatography, liquid-liquid chromatography, ion exchange chromatography, ion pair chromatography, molecular exclusion chromatography, affinity chromatography. Column chromatography, thin layer chromatography (TLC). High performance liquid chromatography (HPLC, UPLC): instrumentation. Enantioselective chromatographic separation using chiral stationary phases.

Gas chromatography (GC): instrumental aspects, types of stationary phase, detection in GC. Capillary electrophoresis (EC): instrumentation, theoretical principles, analytical parameters. Combined techniques: liquid chromatography and photodiode UV-VIS 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). Preparation of samples from complex biological matrices. Validation of the analytical method: linearity, precision, accuracy, reproducibility, limit of detection (LOD), limit of quantification (LOQ). Development of chromatographic methods for quality control of drugs and nutraceuticals in pre-clinical and clinical research. Instrumental food analysis. Determination of drug / target protein interactions, by high performance affinity chromatography, for the development of new drugs.

LABORATORY PRACTICAL CLASSES

Identification of pharmaceutical compounds. Drugs reported in the FUI and Pharm. monographs. Eur. Solubility testing. Acid - basic - amphoteric character. Identification of functional groups. Determination of melting point, refractive index and rotational optical power. Identification of pharmaceutical and nutraceutical-food samples by TLC.

High performance liquid chromatography. Development of an HPLC method for the separation of drugs, nutraceutical, and food in pharmaceutical forms and complex matrices. Study of resolution, selectivity and efficacy by changing chromatographic parameters (stationary phase, mobile phase,, flow, pH and temperature). Calculation of chromatographic parameters (capacity factor, selectivity factor, resolution, number of theoretical plates, peak asymmetry). 

1. Manuale di analisi qualitativa a cura di Giuseppe Caliendo – Edises I/2020 edizione (1 gennaio 2019)

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

3. V. CAVRINI, V. ANDRISANO. Principi di Analisi Farmaceutica. Società Editrice Esculapio, Bologna. IV edizione 2018.

4. R.M. SILVERSTEIN, F.X. WEBSTER: "Identificazione spettroscopica di composti organici" - Ambrosiana Editrice, Milano, 2016 (testo di consultazione).

5. Teaching material provided by the teacher available on Studium.

Verification of learning will be carried out through a final written and/or oral exam.

Verification of learning may also be carried out electronically, should conditions require it.

The calendar of examinations is published on the website of the Department of Pharmaceutical Sciences http://www.dsf.unict.it/corsi/lm-13_ctf/calendario-esami

Describe the identification reactions of pyridine derivatives

Describe the theoretical principles and instrumentation for the determination of specific rotational power

Describe the separation mechanism in partition chromatography

Describe the theoretical principles in capillary electrophoresis