Pharmaceutical Analysis I with Laboratory of Pharmaceutical Analysis I and Food Chemistry

A.Y. 2024/2025
11
Max ECTS
108
Overall hours
SSD
CHIM/08 CHIM/10
Language
Italian
Learning objectives
The course aims to provide students with the knowledge of the main analytical methods and instrumental techniques that are used for the quantitative analysis of drugs both as active substances and in the final medicinal products. In the course we will deepen the theoretical principles that characterize the different methods and mechanisms underlying the functioning of the instruments. Examples of drug dosage applications will be analyzed for a concrete and current understanding of the methods used, and more generally, for a critical examination of the aspects and problems that must be evaluated for the development and validation of an analytical method. In particular, the course aims not only to transfer to the student the knowledge required to understand the analytical methods and their applications for drug analysis according to the current pharmacopoeia, but also to provide useful tools to develop quantitative analytical methods based on the structure of the analytes, the matrix and the required sensitivity. In addition, the course will provide basic notions regarding the composition of foods, emphasizing the characteristics of the main components. In order to make the knowledges provided by the course comprehensible and immediately verifiable, analytical procedures for drug quantitative determination will be applied during practical laboratory exercises, which will allow a concrete understanding of different techniques and the functioning of the analytical instruments.
Expected learning outcomes
At the end of the course the students will have to know the main analytical methods for drugs quantification, their theoretical bases and which classes of drugs they are used for. The students will need to know instrumental dosing techniques, the principles underlying their operation and their applications. Students will have to demonstrate an understanding of the mechanisms, problems and assessments that underlie the choice of the analytical method for the quantitative determination of a drug. During the lectures it will be offered the possibility to apply knowledge and understanding through the proposal of problems that will be solved in the classroom with the involvement of the students. Furthermore, at the end of the course, students will know the composition of different foods, also considering the possible transformations induced by technological treatments and conservation. They will also know some issues related to quality and safety, in particular in relation to the possible presence of contaminants, possible alterations, the main adulterations and the correct use of food additives. The student will have to demonstrate the ability to use the acquired knowledge to develop an analytical method for the quantification of a drug based on the structure and matrix. During laboratory exercises, the student will have to analyze a drug by applying the proposed analytical method and evaluate the results obtained.
Single course

This course can be attended as a single course.

Course syllabus and organization

Linea AK

Lesson period
Second semester
Course syllabus
Teaching unit: Drug Analysis 1
The program of the course is focused on the theory and fundamentals of the practice according to the current European Pharmacopoeia of the following topics:
- Introduction to the principles of quantitative analysis and to the analytical techniques for the analysis of drugs and drug impurities
- Data handling (e.g., margin of error, significant figures, statistical treatment of the experimental errors, statistical tool to compare results with a reference value or with other experimental results).
- Method validation according to the current European Pharmacopoeia or to other international guidelines (e.g., ICH-Q2R2)
- Sample preparation (e.g., sampling, sample storage, liquid-liquid and solid-liquid extractions, evaporation, filtration)
- Materials, equipment and laboratory techniques for quantitative analysis through a direct determination of mass or volume (e.g., scales, volumetric glassware)
- Titrimetry (acid-base titrations, precipitated titrations, redox titrations, complexometric titrations, titrations in non-aqueous solvents, potentiometric titrations).
- Direct potentiometric analyses
- Atomic and molecular UV-Visible Spectroscopy and applications of absorption and emission techniques for quantitative analyses of drugs and drug impurities according to the European Pharmacopoeia
- Chromatographic techniques at ambient pressure (e.g., SPE, TLC), gaschromatography (GC) and high-performance liquid chromatography (HPLC) for the analysis of drugs and drug impurities according to the European Pharmacopoeia

Teaching unit: Laboratory of Drug Analysis 1
- Acid-base titrations: use of colorimetric indicators and potentiometric methods.
- Titrations with formation of precipitate: argentometry.
- Complexometric titrations: direct and inverse.
- Oxidation-reduction titrations: permanganometry, bromometry, iodimetry, iodometry.
- Spectrophotometric determinations: use of external standard calibration method and method of standard additions.

Teaching unit: Food Chemistry
- Organic and inorganic nutrients: macro and microelements, simple sugars, polysaccharides, amino acids, proteins, lipids, minor components, anti-nutritional factors.
- Analysis of the main components of food: water, ash, lipids, reducing and non-reducing sugars, fibers, proteins.
- Non-enzymatic browning: changes induced by industrial and household processes.
- Oils and fats: chemical composition, minor components, hydrolytic and oxidative rancidity, functional properties of polyunsaturated fatty acids; olive oil, technology, refining; main seed oils for food use; analytical problems related to the preservation and sophistication of oils.
- Cereals: caryopsis, chemical composition; differences between wheat and durum wheat, flour, bread and pasta preparation; rice, characteristics and use.
- Milk: chemical composition; diffrences between human milk and cow's milk; milk stabilization, milk analysis. Milk derivatives: cheese, yogurt, ricotta, and butter.
- Additives: legislation and use criteria, toxicological problems; main classes: preservatives, antioxidants, gelling agents, thickeners, emulsifiers, sweeteners, dyes.
- Chemical contamination of natural and human-induced food: heavy metals, PCBs, PAHs, dioxins, agrochemicals, mycotoxins, toxins from bacteria.
Prerequisites for admission
Knowledge of general and inorganic chemistry and stoichiometry and analytical chemistry are required.
The frequency to the Laboratory of Analysis of Drugs 1 is subject to attendance at the Laboratory of Qualitative analysis of inorganic drugs.
The following prerequisites are required to take the exam: it is mandatory to have passed the exam of Analytical Chemistry and it is recommended to have taken the exam Organic Chemistry 1.
Teaching methods
Teaching unit: Drug Analysis 1
Frontal lectures mixed with flipped classrooms

Teaching unit: Laboratory of Drug Analysis 1
Practical exercises in laboratory

Teaching unit: Food Chemistry
Frontal lectures
Teaching Resources
Teaching unit: Drug Analysis 1
Slides and other material published by the teacher on the MyAriel webpage of the course.

Recommended textbooks:
- Skoog, West, Holler: Fundamentals of Analytical Chemistry (second edition) - EdiSes
- Harris D.C.: Quantitative analytical chemistry - Zanichelli
- Hage and Carr: Analytical chemistry and quantitative analysis - Piccin
- Porretta G.C.: Analysis of pharmaceutical preparations. Quantitative analysis - First volume - CISU
- Cavrini V., Andrisano V.: Principles of pharmaceutical analysis - Società Editrice Esculapio

Teaching unit: Laboratory of Drug Analysis 1
The procedures of the laboratory exercises are made available in pdf format on the MyAriel portal of Unimi.

Teaching unit: Food Chemistry
The slides of the course and the scientific literature are provided by the teacher through the MyAriel portal of UNIMI.
Recommended text:
- P. Cabras and A. Martelli: Food Chemistry - Piccin Editore, 2004
Assessment methods and Criteria
For each teaching unit, the learning assessment is evaluated by a test with 30 as the maximum score. The minimum score to pass the tests is 18/30.
The final score is the average of the single scores weighted by the ECTS credits of each teaching unit.

Teaching unit: Drug Analysis 1
During the course anonymous online quizzes will be used as a self-assessment tool for students. During the lectures, some exercises similar to the final test will be discussed as well. Quizzes and exercises will be provided to help the student's understanding.
The final test is a two-hour written test with exercises and short answer questions. The test is aimed at evaluating the knowledge of the theory for the course's topics, the student's ability to solve titrimetric problems, the ability of understand methods reported in European Pharmacopoeia, as well as the ability of designing an approach to analyze a given molecule, based on structural features.
exam consists of a written test which is related to the topics covered in class and is articulated in several points with exercises and open-ended questions with a final grade out of thirty. The written test lasts 120 minutes.
The outcome of the written exam will be published on the MyAriel portal of Unimi.

Teaching unit: Laboratory of Drug Analysis 1
The exam includes ten practical exercises in laboratory. The mark out of thirty is based on the evaluation of errors (e.g., ± 2%) obtained in each practical exercise, the competence in the use of laboratory equipment and the ability to organize and carry out practical work. The outcome will be published on the MyAriel portal of Unimi.

Teaching unit: Food Chemistry
The exam consists of a written test containing multiple choice questions. The outcome will be published on the MyAriel portal of Unimi.
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 8
CHIM/10 - FOOD CHEMISTRY - University credits: 3
Single bench laboratory practical: 40 hours
Lessons: 68 hours

Linea LZ

Responsible
Lesson period
Second semester
Course syllabus
Teaching unit: Drug Analysis 1

The program of the course is focused on the theory and fundamentals of the practice according to the current European Pharmacopoeia of the following topics:

- Introduction to the principles of quantitative analysis and to the analytical techniques for the analysis of drugs and drug impurities

- Data handling (e.g., margin of error, significant figures, statistical treatment of the experimental errors, statistical tool to compare results with a reference value or with other experimental results).

- Method validation according to the current European Pharmacopoeia or to other international guidelines (e.g., ICH-Q2R2)

- Sample preparation (e.g., sampling, sample storage, liquid-liquid and solid-liquid extractions, evaporation, filtration)

- Materials, equipment and laboratory techniques for quantitative analysis through a direct determination of mass or volume (e.g., scales, volumetric glassware)

- Titrimetry (acid-base titrations, precipitated titrations, redox titrations, complexometric titrations, titrations in non-aqueous solvents, potentiometric titrations).

- Direct potentiometric analyses

- Atomic and molecular UV-Visible Spectroscopy and applications of absorption and emission techniques for quantitative analyses of drugs and drug impurities according to the European Pharmacopoeia

- Chromatographic techniques at ambient pressure (e.g., SPE, TLC), gaschromatography (GC) and high-performance liquid chromatography (HPLC) for the analysis of drugs and drug impurities according to the European Pharmacopoeia



Teaching unit: Laboratory of Drug Analysis 1

- Acid-base titrations: use of colorimetric indicators and potentiometric methods.

- Titrations with formation of precipitate: argentometry.

- Complexometric titrations: direct and inverse.

- Oxidation-reduction titrations: permanganometry, bromometry, iodimetry, iodometry.

- Spectrophotometric determinations: use of external standard calibration method and method of standard additions.



Teaching unit: Food Chemistry

- Organic and inorganic nutrients: macro and microelements, simple sugars, polysaccharides, amino acids, proteins, lipids, minor components, anti-nutritional factors.

- Analysis of the main components of food: water, ash, lipids, reducing and non-reducing sugars, fibers, proteins.

- Non-enzymatic browning: changes induced by industrial and household processes.

- Oils and fats: chemical composition, minor components, hydrolytic and oxidative rancidity, functional properties of polyunsaturated fatty acids; olive oil, technology, refining; main seed oils for food use; analytical problems related to the preservation and sophistication of oils.

- Cereals: caryopsis, chemical composition; differences between wheat and durum wheat, flour, bread and pasta preparation; rice, characteristics and use..

- .Milk: chemical composition; diffrences between human milk and cow's milk; milk stabilization, milk analysis. Milk derivatives: cheese, yogurt, ricotta, and butter.

- Additives: legislation and use criteria, toxicological problems; main classes: preservatives, antioxidants, gelling agents, thickeners, emulsifiers, sweeteners, dyes.

- Chemical contamination of natural and human-induced food: heavy metals, PCBs, PAHs, dioxins, agrochemicals, mycotoxins, toxins from bacteria.
Prerequisites for admission
Knowledge of general and inorganic chemistry and stoichiometry and analytical chemistry are required.

The frequency to the Laboratory of Analysis of Drugs 1 is subject to attendance at the Laboratory of Qualitative analysis of inorganic drugs.

The following prerequisites are required to take the exam: it is mandatory to have passed the exam of Analytical Chemistry and it is recommended to have taken the exam Organic Chemistry 1.
Teaching methods
Teaching unit: Drug Analysis 1

Frontal lectures mixed with flipped classrooms



Teaching unit: Laboratory of Drug Analysis 1

Practical exercises in laboratory



Teaching unit: Food Chemistry

Frontal lectures
Teaching Resources
Teaching unit: Drug Analysis 1
Slides and other material published by the teacher on the MyAriel webpage of the course.


Recommended textbooks:
- Skoog, West, Holler: Fundamentals of Analytical Chemistry (second edition) - EdiSes
- Harris D.C.: Quantitative analytical chemistry - Zanichelli
- Hage and Carr: Analytical chemistry and quantitative analysis - Piccin
- Porretta G.C.: Analysis of pharmaceutical preparations. Quantitative analysis - First volume - CISU
- Cavrini V., Andrisano V.: Principles of pharmaceutical analysis - Società Editrice Esculapio

Teaching unit: Laboratory of Drug Analysis 1
The procedures of the laboratory exercises are made available in pdf format on the MyAriel portal of Unimi.

Teaching unit: Food Chemistry
The slides of the course and the scientific literature are provided by the teacher through the MyAriel portal of UNIMI.
Recommended text:
- P. Cabras and A. Martelli: Food Chemistry - Piccin Editore, 2004
Assessment methods and Criteria
For each teaching unit, the learning assessment is evaluated by a test with 30 as the maximum score. The minimum score to pass the tests is 18/30.

The final score is the average of the single scores weighted by the ECTS credits of each teaching unit.



Teaching unit: Drug Analysis 1

During the course anonymous online quizzes will be used as a self-assessment tool for students. During the lectures, some exercises similar to the final test will be discussed as well. Quizzes and exercises will be provided to help the student's understanding.

The final test is a two-hour written test with exercises and short answer questions. The test is aimed at evaluating the knowledge of the theory for the course's topics, the student's ability to solve titrimetric problems, the ability of understand methods reported in European Pharmacopoeia, as well as the ability of designing an approach to analyze a given molecule, based on structural features.

exam consists of a written test which is related to the topics covered in class and is articulated in several points with exercises and open-ended questions with a final grade out of thirty. The written test lasts 120 minutes.

The outcome of the written exam will be published on the MyAriel portal of Unimi.



Teaching unit: Laboratory of Drug Analysis 1

The exam includes ten practical exercises in laboratory. The mark out of thirty is based on the evaluation of errors (e.g., ± 2%) obtained in each practical exercise, the competence in the use of laboratory equipment and the ability to organize and carry out practical work. The outcome will be published on the MyAriel portal of Unimi.



Teaching unit: Food Chemistry

The exam consists of a written test containing multiple choice questions. The outcome will be published on the MyAriel portal of Unimi.
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 8
CHIM/10 - FOOD CHEMISTRY - University credits: 3
Single bench laboratory practical: 40 hours
Lessons: 68 hours
Professor(s)
Reception:
Mon-Fri by appointment
via Luigi Mangiagalli 25, second floor
Reception:
on demand, to be scheduled via email
Via L. Mangiagalli 25, first floor, room 1044