ANALISI FARMACEUTICA E NUTRACEUTICO-ALIMENTARE 2 A - L

Knowledge and understanding. The student will have to acquire theoretical and practical preparation for the identification of organic compounds of pharmaceutical interest as outlined in the monographs of official pharmacopoeias. This involves employing instrumental analytical techniques and chemical assays in solutions in pharmaceutical forms and complex biological matrices. The student should also gain the theoretical basis in the main analytical techniques for the analysis of nutraceuticals and foods in complex matrices.

Application of knowledge and understanding. The student must be able to use the acquired knowledge to develop and validate protocols for the analysis of drugs, nutraceuticals, and foods.

Autonomy of judgment. The student must be capable of interpreting experimental results related to the analysis of active principles present in complex matrices.

Communication skills. At the end of the course, the student should must articulate what they have learned using appropriate terminology for a scientifically accurate presentation concerning analytical techniques and the analysis of compounds of pharmaceutical, nutraceutical, and food interest.

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

Lectures (42 hours) and Laboratory Training (45 hours).

If the course is delivered in a hybrid or remote mode, necessary adjustments may be made as previously declared, in order to adhere to the syllabus and the program.

Information for students with disabilities and/or learning disorders (DSA): To ensure equal opportunities and in compliance with current legislation, interested students can request a personal meeting to plan any compensatory and/or exemptive measures, based on the learning objectives and specific needs. You may also contact the CInAP DSFS faculty representative.

The basic knowledge necessary for the understanding of the course concern: General and Inorganic Chemistry, Organic Chemistry, Physics, and Pharmaceutical and Nutraceutical-Food Analysis 1.

LECTURES

Identification of compounds reported in the Official Italian Pharmacopoeia and the European Pharmacopoeia

Preliminary Tests: Organoleptic characteristics, behavior of substances during combustion, solubility in water and reactive solvents. Classification of substances based on their solubility.

Functional Groups and Tests for Recognition: Carboxylic acids and derivatives, hydroxy acids, phenols, alcohols, aldehydes and ketones, halogen derivatives, amines, nitro compounds. Recognition of carbohydrates and amino acids.

Determination of Physical Constants: Melting point, boiling point, refractive index, optical rotation. Organic elemental analyzers for qualitative-quantitative CHNOS 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; extracolumn factors. Chromatographic peak asymmetry. Resolution.

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, UPLC): instrumentation. Enantioselective chromatographic separations using chiral stationary phases. Gas chromatography (GC): instrumental aspects, types of stationary phases, detection in GC. Capillary Electrophoresis (CE): instrumentation, theoretical principles, analytical parameters.

Combined Techniques: Liquid chromatography and UV-VIS photodiode array 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 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 of pharmaceuticals and nutraceuticals in preclinical and clinical research. Instrumental analysis in the food sector. Determination of drug/target protein interactions using high-performance affinity chromatography (HPAC) for the development of new drugs.

LABORATORY and PRACTICAL CLASSES

Identification of Pharmaceutical Compounds: Drugs listed in the FUI and Pharm. Eur. monographs. Solubility tests. Acid-base-amphoteric character. Identification of functional groups. Determination of melting point, refractometry, and polarimetry. Identification of pharmaceutical and nutraceutical-food samples using TLC. 

High-Performance Liquid Chromatography: Development of HPLC methods for the determination of analytes in pharmaceutical and nutraceutical-food samples present in pharmaceutical forms and complex biological matrices. Study of resolution, selectivity, and efficiency with varying chromatographic parameters (stationary phase, mobile phase, flow rate, pH, and temperature). Calculation of chromatographic parameters (resolution, capacity factor, selectivity factor, 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 materials provided by the teacher.
   

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).

Describe the separation mechanism in partition chromatography.

Describe the theoretical principles of capillary electrophoresis.

Describe the theoretical principles and instrumentation for the determination of specific optical rotation.

Describe the identification reactions of pharmaceutically relevant amines.