LABORATORY OF DRUG ANALYSIS III A - L

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.

EXPECTED RESULTS
Knowledge and understanding. The student will have to acquire the theoretical and practical preparation for the analysis of organic compounds of pharmaceutical interest reported in the monographs of official pharmacopoeias, through specific chemical essays and instrumental analytical techniques.
Applying knowledge and understanding. The student will have to use the knowledge acquired to perform analytical methods that involve analysis in solution and by instrumental chromatographic techniques.
Making judgments. The studentwill have to interpret the experimental results obtained relating to the analysis of unknown mixtures and active principles 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.

Lectures (28 hrs) and laboratory practical classes (28 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.

Learning assessment may also be carried out on line, should the conditions require it.

THEORETICAL 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, amides, esters, lactones, anhydrides, hydroxy acids, phenols, alcohols, aldehydes and ketones, ethers, halogen derivatives, amines, nitrocompounds, aromatic hydrocarbons.

Classes of pharmaceutical compounds, general and specific assays: benzodiazepines, barbiturates, xanthine derivatives, penicillins and cephalosporins, tetracyclines, sulfonamides, alkaloids and narcotic substances, amino acids, carbohydrates, vitamins.

Analytical profile of drug categories: sodium benzoate, sodium salicylate, calcium lactate, calcium pantothenate, acetylsalicylic acid, ascorbic acid, tartaric acid, methyl p-hydroxybenzoate, benzocaine, isoniazid, nicotinamide, sucrose, glucose, fructose, lactose, sulfatiazole, sulfaguanidine, sulfadiazine.

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.

Chromatographic techniques. General principles of the chromatographic process and chromatographic parameters. Theory of chromatographic separations, retention time, efficiency, selectivity, capacity factor, resolution. Van Deemter equation and rate theory. High performance liquid chromatography (HPLC, UPLC), 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.

LABORATORY PRACTICE

Identification of compounds of pharmaceutical interest reported in the Italian and European Pharmacopoeias. Solubility test. Research of acidic, basic and amphoteric character. Identification of functional groups. Determination of the melting point. Identification of unknown drug samples by TLC. Determination of the density of a solid sample 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 specialties.

1. A. Carta, M.G. Mamolo, F. Novelli, S. Piras – Analisi Farmaceutica Qualitativa – Edises 2011.
2. D. G. Watson - Analisi farmaceutica – Edra 2014; D. G. Watson - Analisi Farmaceutica – Edises 2003.
3. V. Cavrini. Principi di Analisi Farmaceutica, terza edizione - Società Editrice Esculapio, Bologna.
4. R.M. Silverstein, F.X. Webster, Identificazione spettroscopica di composti organici - Ambrosiana Editrice, Milano, 2016 (testo di consultazione).