Introduction to the principles and methods of the chemical-pharmaceutical analysis. Qualitative analysis of organic, organometallic and inorganic substances: features and differences. Preliminary examinations: organoleptic test, the relationship between the structure and physicochemical properties.
Analysis of inorganic compounds
Chemical equilibria in solution: solubility; precipitation, fractional precipitation, precipitation in acidic and alkaline environment, colloidal suspensions; solubilization of precipitates. Preliminary tests on inorganic substances. Systematic analysis of anions and cations.
Analysis of organic compounds
Dissolution process and structure-solubility relationships. Classification of organic compounds according to the solubility. Density. Viscosity. Melting point. Eutectic diagrams. Polymorphism. Boiling point. Refractometry. Polarimetry. Resolution of racemates. Analytical procedure for the recognition of pure organic compounds. Preliminary examinations and qualitative elemental analysis. Organic functional analysis: chemical-physical properties, reactivity and assays for recognition of aromatic structures, alkenes, carboxylic acids and derivatives, aldehydes and ketones, alcohols, phenols, amines, carbohydrates and amino acids. Identification tests of xanthines. Crystalline derivatives: selection criteria, preparation of certain classes of derivatives.
Methods of separation and purification
Impurities and their relationship with the chemical structure. Crystallization. Filtration. Purification of ideal and real liquid mixtures. Azeotropes. Distillation. Sublimation. Extraction. Chromatography: principles, techniques and tools. High performance liquid chromatography (HPLC). Basics of HPLC with chiral phases. Gas chromatography. Chromatography with supercritical fluids.
UV and IR qualitative analysis: theory, instrumentation and sample preparation. Nuclear magnetic resonance spectroscopy: general principles and instrumentation. Applications of spectroscopic techniques in the characterization of drugs, the qualitative determination of impurities and stability control.
Pharmacopoeia and Scientific Literature
Illustration and use of the Italian Official Pharmacopoeia, the European Pharmacopoeia and other literature specific for the analysis of the compounds of pharmaceutical interest. Pharmacopoeia monographs. Analysis of cations and anions present in inorganic and organometallic compounds reported in Pharmacopoeia. Identification reactions for classes of organic substances included in the Pharmacopoeia. Analytical procedures for the identification of substances listed in the Pharmacopoeia.
Distinction between inorganic, organo-metallic and organic substances. Organoleptic test. Identification of inorganic compounds according to FU. Organo-metallic substances: assays for the identification of the inorganic cation; recognition of the organic component. Recognition of pure organic compounds: determination of the solubility in water and in organic solvents; assays for the research of the aromatic structure, the unsaturations and the main functional groups. Assays for certain classes of organic compounds of pharmaceutical interest. Separation and identification of organic substances by extraction and TLC; determination of certain physical-chemical properties relevant for analytical purposes. Sublimation. 1HNMR characterization of an organic compound listed in the Pharmacopoeia.