Instrumental analysis of drugs M - Z

Knowledge and understanding: the student will acquire the theoretical and practical skills useful for the identification of organic compounds of pharmaceutical interest, reported in the monographs of the official pharmacopoeias, using instrumental analytical techniques. The student will also acquire the theoretical knowledge of the main analytical techniques for the analysis of active ingredients in biological matrices.

Applying knowledge and understanding. The student must be able to use the knowledge acquired in the context of instrumental analysis to develop and validate analysis protocols for the analysis of active ingredients in pharmaceutical forms and biological matrices.

Making judgements: The student will be able to interpret the experimental results obtained relating to the analysis of active ingredients present in complex matrices.

Communication skills: At the end of the course the student will be able to relate the acquire knowledge with appropriate terminology for a correct scientific presentation focused on analytical techniques and the analysis of compounds of pharmaceutical interest.

Learning skills: The student will develop theoretical/practical skills useful for being able to update and expand his knowledge to face new analytical problems.

Theoretical lessons (35 hours) in the classroom with the aid of video projection systems of slides and videos. Group exercises (12 hours) for small group of students (10-12) on high performance liquid chromatographs (HPLC, HPLC-IEC).

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.

Information for students with disabilities and / or SLD: To guarantee equal opportunities and in compliance with the laws in force, interested students can ask for a personal interview in order to plan any compensatory and / or dispensatory measures, based on the teaching objectives and specifications needs. It is also possible to contact the CInAP contact person (Center for Active and Participatory Integration - Services for Disabilities and / or SLD) of the DEPARTMENT OF DRUG AND HEALTH SCIENCES, Prof. Teresa Musumeci. 

LECTURES
Introduction to instrumental methods of analysis: classification and selection of analytical methods. Chromatographic techniques. General principles of the chromatographic process and chromatographic parameters. Distribution constant. Retention time. Capacity factor. Selectivity. Efficiency: plate theory; van Deemter's equation; extra-column factors. Asymmetry of chromatographic peaks. Resolution. Liquid chromatography: stationary phase, mobile phase. Liquid-solid chromatography, liquid-liquid chromatography, ion exchange chromatography, ion pair chromatography, molecular exclusion chromatography, affinity chromatography. Column chromatography, thin layer chromatography (TLC). High performance liquid chromatography (HPLC): instrumentation. Gas chromatography (GC): instrumental aspects, types of stationary phase, detection in GC. Enatioselective chromatography separation: direct method with use of enantioselective stationary phases; indirect method with derivatization with defined stereochemical reagents. Capillary Electrophoresis (EC): instrumentation, theoretical principles, analytical parameters. Combined techniques: liquid chromatography and UV-VIS photodiode detector (HPLC-DAD), liquid chromatography and mass spectrometry (HPLC-MS), gas chromatography and mass spectrometry (GC-MS). Qualitative and quantitative analysis in HPLC (external and internal standard methods). Sample preparation and extraction methods. Traditional extraction methods (liquid/liquid and liquid/solid). Extraction with supercritical fluids (SFE). Solid phase extraction (SPE). Preparation of samples from complex biological matrices. 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 in pre-clinical and clinical research. Determination of drug/protein interactions, using high performance affinity chromatography (HPAC), useful for the development of new drugs. 

LABORATORY PRACTICAL CLASSES

High performance liquid chromatography: development of an HPLC method for the separation of drugs in complex matrices. Study of efficiency, selectivity, and resolution. Calculation of chromatographic parameters (capacity factor, selectivity factor, resolution, number of theoretical plates, peak asymmetry). Qualitative/quantitative determination of drugs in pharmaceutical forms present on the market.

1.     V. CAVRINI, V. ANDRISANO. Principi di Analisi Farmaceutica. Società Editrice Esculapio, Bologna. IV edizione 2018.

2.     Veronika R. Meyer. Practical High-Performance Liquid Chromatography, 5th Edition. Wiley, New York 2010 (consultation text)

3.     J.F. HOLLER, S.R.CROUCH. Fondamenti di chimica analitica di Skoog e West. EdiSES, III edizione 2015 (consultation text)

4. Teaching material provided by the teacher available on Studium.

1. Describe Thin Layer Chromatography
2. Describe HPLC equipment
3. Describe SPE