Drug analysis 1 and laboratory of drug analysis 1 and food chemistry

A.Y. 2019/2020
12
Max ECTS
120
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 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.
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.
Course syllabus and organization

Linea AK

Lesson period
Second semester
Course syllabus
Teaching unit: Drug Analysis 1
The program of the course includes the presentation and discussion of the following topics:
- Introduction to the principles of quantitative chemical-pharmaceutical analysis.
- Introduction to the analytical techniques used for the quantitative analysis of substances registered in the current European Pharmacopoeia.
- Materials, equipment and laboratory techniques for quantitative chemical-pharmaceutical analysis (the analytical balance, operations for the correct use of the analytical electronic scale, sources of error in weighing, equipment and manipulations connected with weighing, dryers and desiccants, weighing mode, materials for laboratory equipment, equipment for gravimetric and volumetric analysis, calibration of volumetric glassware).
- Treatment and evaluation of statistical data (statistical treatment of experimental error, systematic error, random and gross error, accuracy and precision, sample and population, confidence intervals, Student's t, F test, Q test, analysis of variance, use of spreadsheets in chemical analysis).
- Volumetric analyses and their applications to the quantitative analysis of substances registered in the current European Pharmacopoeia (acid-base titrations, precipitated titrations, redox titrations, complexometric titrations, titrations in non-aqueous solvents, potentiometric titrations).
- Polarography, voltammetry, amperometry.
- UV-Visible Spectroscopy and its applications to the quantitative analysis of drugs according to the European Pharmacopoeia (theoretical principles, molecular orbitals and types of transitions, absorption characteristics of organic compounds, selection rules, instrumentation, absorption law, internal and external standard methods, method of standard additions, mixture analysis).
- Introduction to chromatography analysis (historical outline, classification and chromatographic techniques, chromatogram, distribution constant, retention factor, chromatographic resolution, plate theory, efficiency and selectivity, van Deemter equation, the general elution problem, symmetry of the peaks).
- Gas-chromatography and its applications to the quantitative analysis of drugs according to European Pharmacopoeia (classification of gas-chromatographic techniques, instrumentation and stationary phases, derivatization, quantitative analysis, applications of GC in European Pharmacopoeia, residual solvents).
- High performance liquid chromatography and its applications in the quantitative analysis of drugs according to European Pharmacopoeia (classification of HPLC techniques, stationary and mobile phases, UHPLC and nano-HPLC, instrumentation and detectors, quantitative analysis in HPLC and applications in European Pharmacopoeia) .
- Development and validation of an analytical method (criteria for choosing the optimal analytical method, development and optimization of the instrumental method, validation of the analytical method).
- Sample preparation (sampling, sample preparation and storage, sample preparation techniques, liquid-liquid extraction, liquid-solid extraction, solid phase extraction, experimental and application aspects).
- The principles of Good Laboratory Practice.

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.
- Titrations in non-aqueous solvents: use of colorimetric indicators and potentiometric methods.
- Spectrophotometric determinations: use of external standard calibration method and method of standard additions.
- Statistical treatment of results: average, median, standard deviation, absolute and relative error, confidence intervals; application of t-test, coupled t-test, F test, ANOVA.

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; general information on minor cereals, rye, corn, oats, barley; gluten intolerance and alternative foods.
- Legumes: composition, characteristics of vegetable proteins, health properties, analytical problems.
- 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

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

Teaching unit: Food Chemistry
Frontal lectures
Bibliography
Teaching unit: Drug Analysis 1
All the teaching material presented during the lessons (constituting the topics of the exam) is made available in pdf format on the Ariel portal of Unimi.
Recommended texts:
- 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 Ariel portal of Unimi.

Teaching unit: Food Chemistry
The slides of the course and the scientific literature are provided by the teacher through the Ariel portal of UNIMI.
Recommended text:
- P. Cabras and A. Martelli: Food Chemistry - Piccin Editore, 2004
Assessement methods and criteria
For each of the three teaching units, the learning assessment is evaluated by a mark out of thirty with a minimum grade of 18/30.
The final result will come from the average of the marks obtained in the three teaching units weighted by the credit value of each unit.

Teaching unit: Drug Analysis 1
The 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.
In order to be able to take the examination, it is essential to register for the exam session through the online SIFA service of the University. The outcome of the written exam will be published on the Ariel portal of Unimi.

Teaching unit: Laboratory of Drug Analysis 1
The exam includes twelve practical exercises in laboratory. The mark out of thirty is based on the evaluation of errors (± 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 Ariel 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 Ariel portal of Unimi.
DRUG ANALYSIS 2
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 0
CHIM/10 - FOOD CHEMISTRY - University credits: 0
Lessons: 48 hours
FOOD CHEMISTRY
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 0
CHIM/10 - FOOD CHEMISTRY - University credits: 0
Lessons: 24 hours
Professor: Arnoldi Anna
LABORATORY OF DRUG ANALYSIS 2
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 0
CHIM/10 - FOOD CHEMISTRY - University credits: 0
Single bench laboratory practical: 48 hours

Linea LZ

Responsible
Lesson period
Second semester
Course syllabus
The program of the course includes the presentation and discussion of the following topics:
- Introduction to the principles of quantitative chemical-pharmaceutical analysis.
- Introduction to the analytical techniques used for the quantitative analysis of substances registered in the current European Pharmacopoeia.
- Materials, equipment and laboratory techniques for quantitative chemical-pharmaceutical analysis (the analytical balance, operations for the correct use of the analytical electronic scale, sources of error in weighing, equipment and manipulations connected with weighing, dryers and desiccants, weighing mode, materials for laboratory equipment, equipment for gravimetric and volumetric analysis, calibration of volumetric glassware).
- Treatment and evaluation of statistical data (statistical treatment of experimental error, systematic error, random and gross error, accuracy and precision, sample and population, confidence intervals, Student's t, F test, Q test, analysis of variance, use of spreadsheets in chemical analysis).
- Volumetric analyses and their applications to the quantitative analysis of substances registered in the current European Pharmacopoeia (acid-base titrations, precipitated titrations, redox titrations, complexometric titrations, titrations in non-aqueous solvents, potentiometric titrations).
- Polarography, voltammetry, amperometry.
- UV-Visible Spectroscopy and its applications to the quantitative analysis of drugs according to the European Pharmacopoeia (theoretical principles, molecular orbitals and types of transitions, absorption characteristics of organic compounds, selection rules, instrumentation, absorption law, internal and external standard methods, method of standard additions, mixture analysis).
- Introduction to chromatography analysis (historical outline, classification and chromatographic techniques, chromatogram, distribution constant, retention factor, chromatographic resolution, plate theory, efficiency and selectivity, van Deemter equation, the general elution problem, symmetry of the peaks).
- Gas-chromatography and its applications to the quantitative analysis of drugs according to European Pharmacopoeia (classification of gas-chromatographic techniques, instrumentation and stationary phases, derivatization, quantitative analysis, applications of GC in European Pharmacopoeia, residual solvents).
- High performance liquid chromatography and its applications in the quantitative analysis of drugs according to European Pharmacopoeia (classification of HPLC techniques, stationary and mobile phases, UHPLC and nano-HPLC, instrumentation and detectors, quantitative analysis in HPLC and applications in European Pharmacopoeia) .
- Development and validation of an analytical method (criteria for choosing the optimal analytical method, development and optimization of the instrumental method, validation of the analytical method).
- Sample preparation (sampling, sample preparation and storage, sample preparation techniques, liquid-liquid extraction, liquid-solid extraction, solid phase extraction, experimental and application aspects).
- The principles of Good Laboratory Practice.
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
Frontal lectures
Bibliography
All the teaching material presented during the lessons (constituting the topics of the exam) is made available in pdf format on the Ariel portal of Unimi.
Recommended texts:
- 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
- Antonio Carrieri: Manuale di Analisi Quantitativa dei Medicinali. Edises
- Cavrini V., Andrisano V.: Principles of pharmaceutical analysis - Società Editrice Esculapio
Assessement methods and criteria
The 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.
In order to be able to take the examination, it is essential to register for the exam session through the online SIFA service of the University. The outcome of the written exam will be published on the Ariel portal of Unimi.
DRUG ANALYSIS 2
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 0
CHIM/10 - FOOD CHEMISTRY - University credits: 0
Lessons: 48 hours
Professor: Aldini Giancarlo
FOOD CHEMISTRY
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 0
CHIM/10 - FOOD CHEMISTRY - University credits: 0
Lessons: 24 hours
Professor: Lammi Carmen
LABORATORY OF DRUG ANALYSIS 2
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 0
CHIM/10 - FOOD CHEMISTRY - University credits: 0
Single bench laboratory practical: 48 hours