LABORATORY OF DRUG ANALYSIS III M - Z

Knowledge and understanding. The student will have to acquire the theoretical and practical preparation 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.
Lifelong 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 (28 hrs) and laboratory training (30 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.

Classroom attendance is compulsory. The maximum limit of absences allowed is 30%, as stated in the teaching regulations of the degree course, which can be consulted on the website of the Department of Pharmaceutical and Health Sciences.

The calendar of lectures is published on the website http://www.dsf.unict.it/corsi/lm-13_ctf/orario-delle-lezioni

LECTURES

Identification of compounds registered in the FUI and Pharm. Eur. Separation of mixtures (solvent extraction, crystallisation, distillation, evaporation, filtration, centrifugation). Preliminary assays: organoleptic characters, combustion behaviour of substances, qualitative elemental analysis (Lassaigne assay) and quantitative elemental analysis (CHNS, minimum formula determination). Solubility in water and reactive solvents; classification of substances according to their solubility.

Functional groups and assays for recognition: carboxylic acids, amides, esters, lactones, anhydrides, hydroxy acids, phenols, alcohols, aldehydes and ketones, ethers, halogen derivatives, amines, nitro compounds, aromatic hydrocarbons. Recognition of carbohydrates and amino acids.

Determination of physical constants: melting point, boiling point, density, refractive index, rotational optical power.

Extractive methods for sample preparation. Classical extraction methods (liquid/liquid and liquid/solid). Supercritical fluid extraction (SFE). Solid-phase extraction (SPE). Sample preparation from complex biological and pharmaceutical matrices.

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

Column chromatography, thin layer chromatography (TLC). High performance liquid chromatography (HPLC, UPLC): instrumentation. Ion exchange chromatography (IEC). Molecular exclusion chromatography (GPC, GFC). Affinity chromatography. Determination of drug/target protein interactions using high-performance affinity chromatography (HPAC) for new drug development.

Enatioselective chromatographic separations. Gas chromatography (GC): instrumental aspects, stationary phase types, GC detection. Capillary Electrophoresis (EC): instrumentation, theoretical principles, analytical parameters. 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 in chromatography (external and internal standard methods). Analytical method validation: linearity, precision, accuracy, reproducibility, limit of detection (LOD), limit of quantification (LOQ). 

Development of chromatographic methods for drug assays in quality control and pre-clinical and clinical research. 

LABORATORY PRACTICAL CLASSES

Identification of compounds of pharmaceutical interest reported in the FUI and Pharm. monographs. Eur. Solubility testing. Acid - basic - amphoteric character. Identification of functional groups. Melting point determination. Identification of unknown samples by TLC. Measurement of rotational optical power and enantiomeric excess. Determination of refractive index. Determination of the density of a solid and a liquid sample. Development of analytical methods for the separation of drugs by HPLC. Qualitative/quantitative determination of molecules of pharmaceutical interest in medicinal products. Extraction, purification and characterisation of an active ingredient from a complex matrix.

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 can be found inside the Studium platform.

Written and/or oral examination.

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