LABORATORY OF DRUG ANALYSIS III M - Z

This course is focused on: - the theoretical-practical knowledge for the identification of chemical compounds of pharmaceutical interest reported in the Italian and European Pharmacopoeia (FU, EP) by systematic analysis of organic functional groups and instrumental analytical methods; - the theoretical-practical knowledge of chromatographic separations; - the development of quality control of analitycal methods.

The course includes 28 hours of theoretical lectures and 36 hours of theoretical and practical lessons in the laboratory.

Requirements: knowledge of General and Inorganic Chemistry; knowledge of fundamentals of Organic Chemistry.

Classroom attendance is mandatory. To acquire the frequency signature for the laboratory experiences, the maximum number of absences is 30%.

MANDATORY BOOKING by e-mail to lpasquin@unict.it is required 48 hours before the start date of theoretical lectures. E-mail subject: "Laboratory of Drugs Analysis III (M-Z) reservation".

Assessment: Practical, written and oral exam.

Theoretical part: Identification of the compounds present in Pharmacopea monographies. Separation techniques: solvent extraction, crystallization,distillation, evaporation, centrifugation. Preliminary tests: physical state, colour, odour. Preliminary tests: Combustion behavior of substances, qualitative elementary analysis (Lassaigne assay) and quali-quantitative elementary analysis (CHNS, empirical formula determination). Solubility in water and reactive solvents; The theory of solubility: classification of substances based on their solubility.

Principal functional groups and the reactions used for their identification: carboxylic acids, hydroxy acids, phenols, alcohols, aldehydes and ketones, esters, lactones, anhydrides, ethers, halogen derivatives, amines, amides, nitrocompounds, aromatic hydrocarbons.

General and specific assays on classes of pharmaceutical substances : benzodiazepines, barbiturates, xanthine derivatives, penicillins and cephalosporins, tetracyclines, vitamins, carbohydrates, amino acids, sulfonamides, alkaloids and abuse drugs.

Monographs: benzoic acid, salicylic acid, acetylsalicylic acid, ascorbic acid, tartaric acid, lactic acid, citric acid, methyl p-hydroxybenzoate, benzocaine, paracetamol, isoniazid, nicotinamide, adrenaline, levodopa, methyldopa.

Determination of physical constants: melting point, boiling point, density, refractive index, optical rotatory power. Definition and application of the concept in Pharmacopea.

Extraction and Sample Preparation: Traditional extraction methods (liquid / liquid and liquid / solid). Extraction with supercritical fluids (SFE). Solid phase extraction (SPE). Preparation of samples from complex biological matrices.

Classification and principles of the chromatographic techniques. Chromatographic parameters. Theory of chromatographic separations, retention time, efficiency, selectivity, capacity factor, resolution. Van Deemter equation and rate theory. Thin Layer Chromatography (TLC), High Performance Liquid Chromatography and Ultra High Performance Liquid Chromatography (HPLC, UHPLC), gas chromatography (GC), capillary electrophoresis (EC): definition and practical application of the techniques. Qualitative and quantitative analysis in HPLC (external and internal standard methods). Validation of the analytical method: linearity, precision, accuracy, reproducibility, limit of detection or detention (LOD) and the limit of quantification (LOQ). Development of analytical methods for qualitative and quantitative identification of drugs in quality control and and in pre-clinical and clinical clinical research. Determination of drug/protein interactions, using high performance affinity chromatography (HPAC), for the development of new drugs.

Practice part: the laboratory practice concern the themes treated during the lessons.

1. A. Carta, M.G. Mamolo, F. Novelli, S. Piras – Analisi Farmaceutica Qualitativa – Edises 2011.

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. Teaching material can be found inside the Studium platform.