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Objectives

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.

### Channels

### A - L

### PAOLA CHIMENTI Teacher profile

#### 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

#### Prerequisites

For a better understanding of the theoretical knowledge and technical skills, the student must have learned: - General chemistry, organic chemistry and analitic chemistry, necessary prerequisites for understanding the theoretical knowledge of the extraction methods. - Physics, important prerequisites for understanding the theoretical knowledge of quantitative methods - Maths and Analisi Chimico Farmaceutica e Tossicologica I are useful.

#### Study modes

56 hours lectures will be used to deliver the core material. The practical sessions (60 hours) will complement the material presented in lectures by Individual teaching laboratory lectures.

#### Frequency modes

Practical experiences in the laboratory, with compulsory participation, provide for the active participation of the student in the preparation of solutions with a known concentration, in the treatment of unknown samples, in the execution of volumetric analyzes, in the collection and interpretation of data.

#### Exam modes

The assessment strategy is designed to verify student ability in critically evaluating and representing theoretical and practical knowledge acquired during the course.

Assessment strategy:

- At the end of the teaching laboratory lectures, the student has to prepare a report about the analysis procedure. Self-direction and to act independently will be evaluated. End-of-course exam: written exam. Exercise on quantitative analysis, determination of the absolute or relative abundance of one, several or all particular substance present in a sample

- and evaluation of knowledge of the most common instrumental chemical analysis techniques to determine physicochemical measurements.

The student will be evaluated with a minimum score of 18/30 if he has not achieved mastery of all the topics covered, while knowing how to recognize the different techniques of quantitative analysis; otherwise, the student who has demonstrated that he is able to deal with the quantitative determination of a complex mixture, knowing how to safely choose and decide the most appropriate analytical method among all those addressed, both during the lectures and during the practical laboratory exercises, will be evaluated with a grade of 30/30. If they also have excellent results in the unknown laboratory tests, will be evaluated with 30 and honors.

Elements taken into consideration:

• frequency

• active participation

• language skills

• reasoning skills in both the written and oral tests

• autonomous study skills on the texts indicated

Exam reservation date start | Exam reservation date end | Exam date |
---|---|---|

07/12/2022 | 21/01/2023 | 24/01/2023 |

25/01/2023 | 10/02/2023 | 13/02/2023 |

14/02/2023 | 15/04/2023 | 18/04/2023 |

20/04/2023 | 03/06/2023 | 06/06/2023 |

07/06/2023 | 01/07/2023 | 04/07/2023 |

06/07/2023 | 17/09/2023 | 20/09/2023 |

20/09/2023 | 09/12/2023 | 12/12/2023 |

12/12/2023 | 19/01/2024 | 22/01/2024 |

### M - Z

### ARIANNA GRANESE Teacher profile

#### 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

#### Prerequisites

For a better understanding of the theoretical knowledge and technical skills, the student must have learned: - General chemistry, organic chemistry and analitic chemistry, necessary prerequisites for understanding the theoretical knowledge of the extraction methods. - Physics, important prerequisites for understanding the theoretical knowledge of quantitative methods - Maths and Analisi Chimico Farmaceutica e Tossicologica I are useful.

#### Study modes

56 hours lectures will be used to deliver the core material. The practical sessions will complement the material presented in lectures by Individual teaching laboratory lectures. It will provide guidance and experience of following written experimental procedures and help students to consolidate their practical skills and the subsequent reporting and analysis of practical results.

#### Frequency modes

Pratical session is obligatory

#### Exam modes

Assessment strategy:

- At the end of the teaching laboratory lectures, the student has to prepare a report about the analysis procedure. Self-direction and to act independently will be evaluated. End-of-course exam: written exam. Exercise on quantitative analysis, determination of the absolute or relative abundance of one, several or all particular substance present in a sample and evaluation of knowledge of the most common instrumental chemical analysis techniques to determine physicochemical measurements.

this will be evaluated with a score of 30/30. The latter, if they will have also reported excellent results in the unknown laboratory tests, will be evaluated with 30 cum laude.

- The duration of the written test is one hour, that of the oral exam is about forty minutes.

- The written task includes an exercise on the dosage and quantitative determination of a substance and an open question on an exam topic.

Elements taken into consideration:

• frequency

• active participation

• language skills

• reasoning skills in both the written and oral tests

• autonomous study skills on the texts indicated

Exam reservation date start | Exam reservation date end | Exam date |
---|---|---|

07/01/2023 | 21/01/2023 | 24/01/2023 |

01/02/2023 | 10/02/2023 | 13/02/2023 |

25/03/2023 | 14/04/2023 | 18/04/2023 |

25/05/2023 | 03/06/2023 | 06/06/2023 |

18/06/2023 | 02/07/2023 | 04/07/2023 |

31/08/2023 | 17/09/2023 | 20/09/2023 |

24/11/2023 | 11/12/2023 | 12/12/2023 |

05/01/2024 | 20/01/2024 | 22/01/2024 |

- Academic year: 2022/2023
- Curriculum: Curriculum unico
- Year: Third year
- Semester: First semester
- SSD: CHIM/08
- CFU: 10

- Attività formative caratterizzanti
- Ambito disciplinare: Discipline Chimiche, Farmaceutiche e Tecnologiche
- Lecture (Hours): 56
- Lab (Hours): 60
- CFU: 10
- SSD: CHIM/08