The course is dedicated to the study of methods relating to the extraction, purification, separation, identification and qualitative-quantitative instrumental analysis of active ingredients present in pharmaceutical formulations. The course is divided into theoretical lessons and practical laboratory single-seat exercises.
Testi di riferimento
Principi di Analisi Farmaceutica – V. Cavrini, V. Andrisano, Ed. Esculapio
Chimica Analitica Strumentale - D. A. Skoog, J. J. Leary, Ed. Edises
Analisi Chimica Strumentale B e C - R. Cozzi, P. Protti, T. Ruaro, Ed. Zanichelli
Analisi Chimica Cromatografica - E. Mentasti, G. Saini, Ed. Piccin
Analisi farmaceutica - D. G .Watson, Ed. Edises
Chimica analitica quantitativa - D.C. Harris, Ed. Zanichelli
Learning Objectives
The aim of the course is to perfect laboratory practice, recalling information on safety rules and the correct handling of reagents and solvents. Knowledge is also provided to apply, with the appropriate glassware and instrumentation, methods relating to the extraction, purification, separation and instrumental quantification of active ingredients present in pharmaceutical formulations. The course is divided into theoretical lessons and practical laboratory exercises in single place, to which ample space is dedicated.
At the end of the course the student will have developed:
- the ability to apply classical and/or instrumental chemical methods to the purification, separation and quantification of substances of pharmaceutical interest, of natural and/or synthetic origin, present in matrices of various kinds.
- the ability to analyze, elaborate, interpret and evaluate the significance of the results obtained experimentally;
- awareness of the rules in chemical laboratories, of the aspects of safety and waste disposal and of the risks associated with the instruments used.
Prerequisites
Attendance at the course is compulsory (Directive 85/432/EEC); the minimum frequency required is 90% (Regulations of the CdS). To attend the course it is necessary to have attended Analytical Chemistry, Drug Analysis I, II, III and to be in possession of safety training (4 hours general training + 12 hours specific risk). Information on this can be found on the website of the CdS and the School of Human Health Sciences.
Before taking the exam for this course, the student must have successfully passed the Analytical Chemistry, Drug Analysis I, II, III exams. It is also recommended to take Organic Chemistry.
Teaching Methods
The course will be divided in lectures (3 CFU) and laboratory exercises in single place (3 CFU). Each exercise is preceded by a theoretical lesson where the operating instructions for the next exercise are given.
The teaching material and some audio recordings explaining laboratory activities will be uploaded to the Moodle e-learning platform (https://e-l.unifi.it) available to students. The lessons will take place via video projection while the appropriate instruments and equipment will be provided for the exercises.
Further information
Office hours: every day, by appointment Department of NEUROFARBA, Section of Pharmaceutical and Nutraceutical Sciences
Via U. Schiff, 6 - 50019 Sesto F.no - Florence
e-mail: silvia.dei@unifi.it
e-mail: gianluca.bartolucci@unifi.it
Type of Assessment
The exam consists of a written test (lasting 60 minutes) which focuses on all topics: lectures and laboratory exercises. The test can be taken during any exam session shown on the University Exam Booking Service page, subject to compliance with the prerequisites, and consists of various types of questions: open answer/multiple choice/problem solving. In the exam, the student demonstrates the knowledge and understanding acquired by applying them to the resolution of exercises (about 35% of which contributes to the formation of the grade) and the ability to process and communicate the knowledge and tools acquired during the course ( 35%) using appropriate scientific language (30%). The final grade results from all these contributions considered important indicators of the adequacy of the level of learning achieved and of the achievement of the results envisaged by the course.
Course program
Rules of conduct in the laboratory and the CLP regulation for the use of chemicals and their mixtures; training.
Analytical method for the search for organic substances: sample homogenization, analyte extraction, purification and analytical determination.
Sample preparation: static and dynamic headspace, liquid-liquid extraction (LLE), solid phase extraction (SPE), solid phase microextraction (SPME).
Purification of the extracted sample: filtration, centrifugation, distillation (simple, fractional, steam current, reduced pressure), crystallization, sublimation.
Introduction to chromatographic techniques: quantities, equations, fundamental parameters, plate theory and dynamic theory.
Chromatographic techniques: planar chromatography (TLC), liquid chromatography on column, HPLC, GC.
Quantitative chromatography: measurement of the area of the chromatographic peak and methods of analysis.
The single-seat laboratory exercises involve the application of some extraction techniques and qualitative and/or quantitative chromatographic determinations.