Catalogo dei Corsi di studio

General expected learning outcomes
The aim of Analisi Chimico Farmaceutica e Tossicologica II course is to contribute knowledge and ability about the quantitative determination of drugs and substances of pharmaceutical interest, as well as to make students aware of the importance of safety in experimental practice.

Specific expected learning outcomes
1. Knowlwdge and understanding
The students at the end of the course will have competences necessaries for analysis of organic and inorganic compounds, they’ll learn the techniques of volumetric, gravimetric, chromatographic and spectrophotometric analysis, they will choose the method for determining the substance and study the concept of error for the determination of analytical data.

2. Applying knowledge and understanding
At the end of the course the student will be able to prepare solutions with a known concentration, perform calculations to determine the analyte content in unknown samples, choose the appropriate volumetric analysis method and know the optimal operating conditions, will be able to interpret the monographs present in the European Pharmacopoeia.

3. Making judgements
The student attends individual teaching laboratory lectures where he applies quantitative determination methods to pharmaceutical products. Self-direction and to act independently to a level where the student has a practical understanding of the learned techniques. At the end of each laboratory lecture the student has to prepare a report about the analysis procedure. Moreover, during the final test the student will exercise on mixture separation.

4. Communication skills
The student, thanks to the tests carried out during the laboratory, will demonstrate that he has acquired the ability to determine the quantity and purity of the compounds through a test and a subsequent oral interview. These skills will be specifically valued during practical laboratory.

5. Learning skills
The student will be able to independently learn all the analytical techniques thanks to the availability of texts and handouts; furthermore, he can complete the study using his own notebook written in the laboratory.

Programme

INTRODUCTION: chemical equilibrium and concepts of solubility, ionic strength, activity, activity coefficient, concentration. (2 hours)
VOLUMETRIC ANALYSIS: general information on Equivalence and titration reactions. Practical aspects in volumetric analysis: instrumentation and laboratory glassware. Acid - base titrations: titration curves of acids and bases.(2 hours) Determination of the end point of the titration: acid-base indicators. Practical aspects: primary standards and applications. Acid - base titration in aqueous-organic solvents. (4 hours)
Acid – base titrations in non-aqueous medium: autoprotolysis and acid - base solvents; dielectric constant.Equilibria in glacial acetic acid and titration of weak bases with examples by the pharmacopoeias; (4 hours)
titration of weak acids in non-aqueous medium with examples by the pharmacopoeias. (2 hours)
Precipitation titrations: Titration curves. Argentometric methods (Mohr, Fajans, Volhard methods). Applications. (2 hours)
Complex-formation titrations: titration with EDTA. Indicators for EDTA titrations; applications. (4 hours)
Redox titrations: Overview of oxidizing and reducing agents. Scale of redox potentials and Nernst equation. Redox titration curves and applications.(6 hours)
ELECTROCHEMICAL METHODS OF ANALYSIS:
Potentiometry. General principles, electrodes and definition of standard reduction potentials. Electrochemical cells as analytical probes. Most common electrodes: reference electrodes and indicator electrodes. Glass electrode for pH measuring and other selective electrodes. Potentiometric titrations and examples of applications of the pharmacopoeias. ( 6 hours)
Conductimetry:Theoretical principles on the conductivity of electrolytes. Conductivity cell. Conductimetric titrations: examples of applications.(2 hours)
PRINCIPLES OF STATISTICS FOR THE EVALUATION OF ANALYTICAL DATA: Measurement and error (systematic and random). Application of basic statistical knowledge (mean, standard deviation, variance, normal or Gaussian distribution, Student's t distribution etc..) to real analytical results. (2 hours)
QUANTITATIVE ANALYSIS BY UV-vis SPECTROPHOTOMETRY: Theoretical principles of UV-vis absorption. Beer-Lambert law. Constituent elements of spectrophotometers (single and double beam). Applications: analysis of binary mixtures; differential spectrophotometry; derivative spectrophotometry. Chromogenic derivatization methods. Applications to the analysis of drugs and examples by the pharmacopoeias. (6 hours)
HPLC and GC (6 hours)
SAFETY IN LABORATORY: Behavior in lab and risks arising from handling chemicals.
Gravimetric analysis Quantitation by calibration curves of active ingredients in pharmaceuticals. (2 hours)
Exercises (8 hours)

Adopted texts

• Giulio Cesare PORRETTA: Analisi di preparazioni farmaceutiche. Analisi quantitativa. ED CISU
• Mariangela Biava, Rossella Fioravanti, Giulio Cesare Porretta: esercizi di analisi quantitativa di composti farmaceutici. Ed Cisu
• Enrico Abignente Daniela Melisi Esercizi di Analisi Farmaceutica di Composti Farmaceutici. Ed CISU
• Skoog, West, Holler, Fondamenti di Chimica Analitica, Ed Edises
• Hage , Carr: Chimica analitica e analisi quantitativa. Ed Piccin
• M. Grazia Rimoli: Principi di Analisi quantitativa dei medicinali. ED Loghia teoria, pratica, eserciziario
• Cavrini Andrisano Principi di analisi farmaceutica, editrice esculapio

Programme

INTRODUCTION: chemical equilibrium and concepts of solubility, ionic strength, activity, activity coefficient, concentration.
VOLUMETRIC ANALYSIS: general information on Equivalence and titration reactions. Practical aspects in volumetric analysis: instrumentation and laboratory glassware. Acid - base titrations: titration curves of acids and bases (2 hours). Determination of the end point of the titration: acid-base indicators. Practical aspects: primary standards and applications. Acid - base titration in aqueous-organic solvents (2 hours).
Acid – base titrations in non-aqueous medium: autoprotolysis and acid - base solvents; dielectric constant.Equilibria in glacial acetic acid and titration of weak bases with examples by the pharmacopoeias; titration of weak acids in non-aqueous medium with examples by the pharmacopoeias.
Precipitation titrations: Titration curves. Argentometric methods (Mohr, Fajans, Volhard methods). Applications.
Complex-formation titrations: titration with EDTA. Indicators for EDTA titrations; applications.
Redox titrations: Overview of oxidizing and reducing agents. Scale of redox potentials and Nernst equation. Redox titration curves and applications (6 hours).
ELECTROCHEMICAL METHODS OF ANALYSIS:
Potentiometry. General principles, electrodes and definition of standard reduction potentials. Electrochemical cells as analytical probes. Most common electrodes: reference electrodes and indicator electrodes. Glass electrode for pH measuring and other selective electrodes. Potentiometric titrations and examples of applications of the pharmacopoeias (6 hours).
Conductimetry:Theoretical principles on the conductivity of electrolytes. Conductivity cell. Conductimetric titrations: examples of applications (2 hours).
PRINCIPLES OF STATISTICS FOR THE EVALUATION OF ANALYTICAL DATA: Measurement and error (systematic and random). Application of basic statistical knowledge (mean, standard deviation, variance, normal or Gaussian distribution, Student's t distribution etc..) to real analytical results (2 hours).
QUANTITATIVE ANALYSIS BY UV-vis SPECTROPHOTOMETRY: Theoretical principles of UV-vis absorption. Beer-Lambert law. Constituent elements of spectrophotometers (single and double beam). Applications: analysis of binary mixtures; differential spectrophotometry; derivative spectrophotometry (6 hours). Chromogenic derivatization methods. Applications to the analysis of drugs and examples by the pharmacopoeias.
HPLC (4 hours)
SAFETY IN LABORATORY: Behavior in lab and risks arising from handling chemicals.
Quantitation by calibration curves of active ingredients in pharmaceuticals (8 hours).

Adopted texts

• Giulio Cesare PORRETTA: Analisi di preparazioni farmaceutiche. Analisi quantitativa. ED CISU
• Mariangela Biava, Rossella Fioravanti, Giulio Cesare Porretta: esercizi di analisi quantitativa di composti farmaceutici. Ed Cisu
• Enrico Abignente Daniela Melisi Esercizi di Analisi Farmaceutica di Composti Farmaceutici. Ed CISU
• Skoog, West, Holler, Fondamenti di Chimica Analitica, Ed Edises
• Hage , Carr: Chimica analitica e analisi quantitativa. Ed Piccin
• M. Grazia Rimoli: Principi di Analisi quantitativa dei medicinali. ED Loghia teoria, pratica, eserciziario
• Cavrini Andrisano Principi di analisi farmaceutica, editrice esculapio