00012 - DRUG ANALYSIS II (A-G)

Introduction to Pharmaceutical Analysis
analysis officers, the Italian and European Official Pharmacopoeia
Safety Standards and Laboratory Equipment
Sources of risk, chemical reagents, rules of conduct, materials and instrumental equipment
Determination of the chemical-physical parameters
Melting point, freezing point, melting point. Refractive index and rotational power.
Methods of Separation and Purification of Active Ingredients
Crystallization, sublimation, distillation, extraction methods, drying and separation of mixtures
Chromatographic Methods: historical notes, classification and instrumentation
Column and thin layer chromatography, paper and ion exchange chromatography. The separative process, retention time and volume, characteristics of the chromatographic peak, capacity factor, selectivity, efficiency, theoretical plate and height of the theoretical plate, resolution equation.
Liquid phase chromatography of adsorption, adsorption isotherms, fixed and mobile phases, elution modes. Distribution chromatography. Thin layer chromatography. Diffusion effects and Van Deemter equation.
Gas chromatography: carrier gas, types of columns, stationary phases, van Deemter equation, temperature effect, instrument, detectors: thermal conductivity, flame ionization, electron capture.
High performance liquid chromatography HPLC: normal and inverse bound phases, sample introduction, pumps, detectors: refractive index, UV spectrophotometric, fluorescence.
Refractometry and Polarimetry
Absolute and relative refractive index, critical angle and limit angle, Abbé refractometer. Concept of chirality, polarized light, Nicol prism, factors that affect optical activity, specific rotational power, applications in the pharmaceutical field.
Spectroscopic Methods
Introduction, UV spectrophotometry: binding and antibonding orbitals, chromophores, bathchromic, hyperchromic, ispochromic and hypochromic effects, Lambert-Beer law, instrument, direct and indirect applications in the pharmaceutical field. IR spectrophotometry: harmonic and anharmonic oscillator, vibratory motions, absorption frequencies of the main functional groups, instrument, applications in the pharmaceutical field.
NMR nuclear magnetic resonance spectroscopy: characteristics of nuclei, nuclear spins, angular and magnetic momentum, precession of a nucleus, types of magnets, description of nuclear magnetic resonance, conditions for the occurrence of resonance, spin-spin and spin-relaxation processes lattice, causes of chemical displacement: inductive effect and magnetic anisotropy, conditions for the equivalence of chemical displacement, spin-spin coupling, coupling constant, first and higher order spectra, two-spin systems AB, AM and AX, three-spin systems AMX and ABC, four-spin systems AA'BB 'and AA'XX', double resonance techniques. Interpretation of first order spectra.
Inorganic Qualitative Analysis
Explanation of the basic techniques and operations to be carried out in the laboratory: solubilization, dilution, precipitation, filtration, centrifugation, calcination. Dry analysis: platinum wire assay, earthenware assay. Chemical-physical, toxicological characteristics and analytical reactions of the main cations and anions with reference to the medicaments listed in the Official Pharmacopoeia: iodine, sulfur, coal, carbon monoxide, hydrogen peroxide. Trace analysis (limit assays) Execution of practical exercises in a single place that focus on applying the main analytical-qualitative reactions for each chemical species studied. Analytical recognition of inorganic substances of pharmaceutical interest both dry and wet
Organic Qualitative Analysis
Preliminary tests: organoleptic test, combustion tests, solubility, behavior of the substance. Qualitative research of the following elements: carbon, nitrogen, sulfur, halogens. Characterization of the following functional groups: Hydroxyl function (alcohols, glycols, carbohydrates and phenols); Ethereal function; Carbonyl function (aldehydes and ketones); Carboxyl function (acids and derivatives); Amine function; Amide function; Nitro-derivatives; Amino acids; Halogen derivatives; Search for unsaturation and aromatic structure.
Specific recognition assays for: acetates, citrates, tartrates, lactates, benzoates, salicylates, xanthine derivatives, aminobenzosulphonamides and sugars.
Practical exercises on the recognition of inorganic, organometallic and organic medicaments registered in the FU
Flame tests, wet tests, calcification residue analysis and specific tests for the identification of the inorganic and / or organic component. Determination of solubility in water and organic solvents.
Assays for the recognition of unsaturation, aromatic structure and functional groups. Separation of organic substances in mixture by means of extraction techniques, TLC. Identification of unknown substances.