LABORATORY OF DRUG ANALYSIS III M - Z

At the end of the course the student: - acquires the theoretical and practical knowledge for the identification of compounds of pharmaceutical interest, reported in the official pharmacopoeias (italian
and european), through specific chemical essays and instrumental analytical techniques; - acquires theoretical and practical knowledge of chromatographic separations; - will be able to apply the acquired knowledge for the development of chromatographic methods for the quali-quantitative identification of drugs in quality control, in medicinal chemistry and in pre-clinical and clinical research.

The course includes 28 hours of lectures and 36 hours of laboratory practical classes.

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.

LESSONS

Identification of drug substances reported in the Italian and European pharmacopoeias. Methods of mixture separation (solvent extraction, crystallization, distillation, evaporation, filtration, centrifugation). Preliminary tests: physical state, colour, odour. Combustion behavior of substances, qualitative elementary analysis (Lassaigne assay) and quali-quantitative elementary analysis (CHNS, empirical formula determination). Solubility in water and reactive solvents; classification of substances based on their solubility.

Identification of drugs by chemical reactivity of functional groups: carboxylic acids, hydroxy acids, phenols, alcohols, aldehydes and ketones, esters, lactones, anhydrides, ethers, halogen derivatives, amines, amides, nitrocompounds, aromatic hydrocarbons.

Classes of pharmaceutical compounds, 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.

Physical chemical constant determination. Melting point of crystal drugs and boiling point of liquid drugs. Refractive index determination by Abbe refractometer. Specific optical rotatory power and polarimetric determination. Density. Determination of relative density of solids and liquids.

Extraction methods for sample pretreatment. Traditional extraction methods (liquid/liquid and liquid/solid). Extraction with supercritical fluids (SFE). Solid phase extraction (SPE). Preparation of samples from complex biological and pharmaceutical 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): instrumentation, theoretical principles, analytical parameters.

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. 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.