| Code |
A001743 |
| Location |
PERUGIA |
| CFU |
5 |
| Teacher |
Giuseppe Manfroni |
| Teachers |
|
| Hours |
- 55 ore - Giuseppe Manfroni
|
| Learning activities |
Caratterizzante |
| Area |
Discipline chimiche, farmaceutiche e tecnologiche |
| Sector |
CHIM/08 |
| Type of study-unit |
Obbligatorio (Required) |
| Language of instruction |
Italian |
| Contents |
A theoretical and practical overview of the main instrumental techniques used to identify and characterise organic molecules, drugs, and healthcare products. |
| Reference texts |
V. Cavrini, V. Andrisano. Principi di Analisi Farmaceutica IV Edizione. Esculapio. Testi per la consultazione: Holler, Skoog, Crouch. Chimica Analitica Strumentale II ed. EDISES K.A. Rubinson, J.F. Rubinson. Chimica Analitica Strumentale. Zanichelli |
| Educational objectives |
On completing the Analysis of Drugs and Health Products II module, students will have acquired the fundamental concepts of instrumental analysis applied to the assay and dispensing of drugs and products used in healthcare. The course covers the following topics: light-matter interaction; the origin and interpretation of UV, IR and NMR (1H and 13C) spectra; the effect of solvents on instrumental techniques; and basic instrumentation. Polarimetric and refractometric instrumental analyses. Theoretical and practical basis for using X-ray diffraction and electron microscopy techniques in the structural and morphological characterization of drugs in order to understand the physical principles of the techniques, interpret experimental data, and evaluate the information obtained in terms of crystal shape, morphology, and purity. Skills: interpreting simple spectra of organic molecules and choosing appropriate instrumental methods for structure confirmation, assaying and estimating the purity of a given drug sample. During the practical sessions, students will learn to use the essential instrumentation required for instrumental analysis. |
| Prerequisites |
Before attending the teaching modules for Drug Analysis II (Module I), students must meet the following prerequisites: It is essential to understand the topics covered in the General and Analytical Chemistry course, and students are expected to be familiar with the fundamental concepts of physics, such as electromagnetism and optics, the corpuscular and wave theories of light, and classical mechanics. Other prerequisites for successfully attending the course relate to organic chemistry, including nomenclature and knowledge of functional groups and their reactivity and reaction mechanisms. |
| Teaching methods |
Lectures with video-projected explanatory slides and an opportunity to actively interact with the lecturer by asking questions and offering critical insights. There will be exercises on the interpretation of NMR, IR, UV and XRD spectra. Practical and theoretical exercises will be organised during the semester and before exam sessions as part of integrated teaching. |
| Other information |
Practical and theoretical exercises will be organized during the semester and before the exam sessions. These activities are within the supplementary teaching activity. |
| Learning verification modality |
The oral exam will be essentially focused on four open questions and will be aimed at verifying that the student is capable of arguing the answer to a particular question in a competent, punctual, clear but synthetic way. The student must demonstrate that it has acquired the skills and abilities required by the course. For the course of Analysis of Medicines III, the oral examination provides that the student is capable of interpreting NMR and IR spectrum of simple organic molecules or drugs. Students with disabilities are invited to visit the following link: http://www.unipg.it/disabilita-e-dsa |
| Extended program |
Introduction to the course: teaching method, role and importance of instrumental techniques for the Pharmaceutical Analysis, the European and Italian Pharmacopoeias, monographs of drugs and instrumental analysis herein reported. Light-matter interaction: corpuscolar-ondulatory theory of light, wavelength, frequency and energy, light speed on to materials with different density, absorption, emission, photoluminescence, electromagnetic spectrum and associated instrumental analyses. Refractometric technique: light speed on to materials with different density; definition and meaning of the refractive index; geometric definition, absolute and relative indices of refraction, determination of the limit angle, parameters that affect the refractive index, Abbe refractometer. Polarimetric technique: concept of chirality and asymmetry of molecules, symmetry operations in molecules that do not possess chiral centers, polarized light and Nicol's prism, light-matter interaction (circularly polarized light components on the floor), Fresnel's law, optical specific rotation angle in the Pharmacopoeia, parameters affecting the deflection angle of polarized light, polarimeter. UV spectroscopy: the Beer-Lambert's law and deviations from linearity; the concepts of absorbance and transmittance; the molar absorptivity coefficient; electronic transitions; their significance and energies involved (HOMO-LUMO transitions), concepts of the chromophore and auxochrome; conjugation effect; effect of the solvent, the statistical probability of transition and extension of the chromophore as factors influencing the molar absorptivity coefficient, influence of pH on auxochromes, sample preparation, instrumentation. IR spectroscopy: harmonic and anharmonic oscillators, Hooke's law; the vibrational quantum number; electric dipole moment; general conditions for the absorption of IR radiation; degrees of vibrational modes for linear and no-linear molecules; frequency of stretching and bending of the main bonds; overtones and combination bands; inactive IR absorption; sample preparation and use of solvents; instrumentation and analysis of spectra of simple organic molecules and drugs. Nuclear magnetic resonance spectrometry: Historical milestones of NMR; properties of nuclei with magnetic spin; the concept of magnetic resonance (Larmor frequency and radiation incident on core precession); the effect of a magnetic field on spin populations; the concept of chemical shift and the use of TMS as a reference molecule; spin–spin coupling and coupling constants; magnetic spin multiplicity. First and second order spectra; AM, AX, A2X3 and AA'XX', AA'BB' systems; the use of deuterated water; H-H and H-F coupling constants; the diagnostic significance of coupling constants in determining molecular structure; the magnets employed in NMR; Fourier spectrum acquisition (pulse NMR); instrumentation; and spectra of simple organic molecules and drugs. NMR of carbon-13: general aspects and conditions of 13C resonance, H-C totally coupled spectra and decoupling, methods for recording a 13C spectrum, JMOD spectra and the chemical shifts of carbons in main functional groups and molecular portions, and C-F coupling and coupling constants. Spectra of simple organic molecules and drugs. Amorphous state and crystalline state. Pharmaceutical polymorphism and its importance for bioavailability, stability, and technological properties. Elemental cells, Bravais lattices, Miller indices, crystal symmetries. Crystalline systems relevant to organic molecules. Radiation/matter interaction. Bragg's law. Qualitative analysis and phase identification. Effects of disorder, broad peaks, presence of amorphous. Examples of polymorph identification. Instrumental geometries: Bragg-Brentan. Sampling, sample preparation. Reading and interpretation of a diffractogram of a drug substance. Electron-matter interaction, generation of secondary and backscattered electrons. Morphological analysis of APIs, co-crystals, hydrated forms. Study of surfaces, porosity and particle aggregation. Examples of SEM and TEM analysis. Elemental microanalysis (EDX) as a complementary tool. Presentation of real examples from scientific literature or pharmaceutical industry: identification of a polymorph by XRD; comparison of two formulations with different morphology by SEM. |
| Obiettivi Agenda 2030 per lo sviluppo sostenibile |
Development of sustainable methods of drug analysis. Application of green chemistry principles in instrumental analysis techniques. |
