Principles of quantitative pharmaceutical analysis and Laboratory for quantitative analysis

A.Y. 2019/2020
8
Max ECTS
80
Overall hours
SSD
CHIM/08
Language
Italian
Learning objectives
Two didactic units composes the course: lectures (Principles of Quantitative Pharmaceutical Analysis) and individual laboratory training (Laboratory for Quantitative Analysis).
The objectives of the lectures consist in providing the knowledge needed to apply the analytical methods, already partially learned in the preparatory courses (General and Inorganic Chemistry, and Stoichiometry, Analytical Chemistry and Inorganic Analysis of Substances having Pharmaceutical Interest and Qualitative Analysis Laboratory), described in the current European Pharmacopoeia for the quantitative analysis of substances for pharmaceutical use.
Concerning the experimental practices, the students will acquire the skills needed for the dosage of pharmaceutical substances reported in the Italian and European Pharmacopoeias.
Expected learning outcomes
By the lectures, the students will have improved further their knowledge concerning the theoretical and practical aspects related to the quantitative analysis, which they will have applied during the individual experimental practices.
The laboratory experiences (mandatory) will have provided to the students the skills to perform the quantitative analysis of pharmaceutical compounds, to complete their knowledge (by means also of other courses as Assays and Methods of Analysis of the Pharmacopoeias and Laboratory of Drug Identification), needed to take the qualifying examination of Pharmacist.
Course syllabus and organization

Linea AL

Responsible
Lesson period
Second semester
Course syllabus
Principles of Quantitative Pharmaceutical Analysis (Lessons)
Introduction to the principles of medicinal chemical- quantitative analysis.
The current European pharmacopea as a reference text for quantitative analyses of active ingredients, excipients, plant extracts and nutrients.
Statistical processing and evaluation of analytical data.
Development and validation of an analytical method.
Gravimetric analysis.
Volumetric analysis: Definition of direct titrations, back- and indirect-titrations; acid-base titrations; precipitation-forming titration, oxidation-reduction titrations; complex-formation titrations; potentiometric titrations - nonaqueous titrations.
Analytical techniques described in the current European Pharmacopea applied to quantitative analysis.
Introduction to analytical techniques; Potentiometry; voltammetry; amperometry; optical methods; UV-Visible spectroscopy, fluorescence and phosphorescence; chromatography techniques; high-performance liquid chromatography; gas-chromatography and Headspace analysis.
Program of the practical laboratory experiences:
- Illustration of the analytical laboratory hardware (e.g. glassware, instruments, etc.);
- complexation titrations;
- oxidation-reduction titration (permanganometry, iodimetry, Iodometry .
- acid- base titrations;
- precipitation titrations.
Prerequisites for admission
The student must have a good knowledge of General and Analytical Chemistry and, in particular, of the chemical solution equilibriums.
Teaching methods
Lectures and laboratory experiences (mandatory).
Teaching Resources
All information about the program and educational materials (slide) is present on the teacher's ARIEL website.
Recommended Books:
Chimica analitica quantitativa - D. C. Harris - Zanichelli
Chimica analitica - Skoog, West, Holler - EdiSES
Chimica analitica e analisi quantitativa - D. S. Hage, J. D. Carr - Piccin
Principi di Analisi Farmaceutica - Cavrini V. Andrisano V. - Esculapio 2017
Analisi strumentale - Bauer, Christian, O'Reilly - Piccin
Analisi di preparazioni farmaceutiche -Giulio Cesare Porretta - CISU
Vogel's Textbook of quantitative Chemical analysis - Longman Eds
European Pharmacopoeia Online - EDQM website
Assessment methods and Criteria
The verification of the learning is carried out by a written test and subsequent oral test.
The examination consists of a written test based on the resolution of problems related to the stechiometry and the chemical equilibrium of the various titration's reactions. The passing of the writing will allow access to the oral examination in which will be evaluated the real competences of the student regarding the theory of quantitative analysis, the application of the various analytical methods and above all of critical evaluation of the analytical data.
Laboratory for quantitative analysis
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 2
Single bench laboratory practical: 32 hours
Shifts:
Turno 2
Professor: Straniero Valentina
Principles of quantitative pharmaceutical analysis
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 6
Lessons: 48 hours
Professor: Valoti Ermanno

Linea MZ

Responsible
Lesson period
Second semester
Course syllabus
Program of the lectures:
- Statistical data analysis applied to analytical chemistry.
- Introduction of the principles of the analytical chemistry applied to pharmaceutical substances.
- Volumetric analysis applied to the quantitative evaluation of the substances included into the European Pharmacopeia:
- neutralization titrations;
- precipitation titrations;
- complexation titrations;
- redox titrations;
- titrations in non-aqueous solvents.
- Introduction to the instrumental techniques for the quantitative analysis:
- UV-vis spectroscopy;
- Gas-chromatography;
- Liquid chromatography.
- Techniques for sample preparation.
- Development and validation of an analytical method.

Program of the practical laboratory experiences:
- hardware of the analytical laboratory (e.g. glassware, instruments, etc.);
- complexation titrations;
- redox titrations: permanganometry and iodimetry.
- neutralization titrations;
- precipitation titrations.
Prerequisites for admission
Knowledge of general chemistry, analytical chemistry and qualitative chemical inorganic analysis is required for this course. Furthermore, for the laboratory training (Laboratory for Quantitative Analysis) the student must have already attended the course of Qualitative Analysis Laboratory (second year).
Teaching methods
The course includes both lectures (Principles of Quantitative Pharmaceutical Analysis unit) and practical laboratory experiences (Laboratory for Quantitative Analysis unit).
During the practical sessions, specific didactic material is provided in electronic format.
Teaching Resources
Recommended books:

Giulio Cesare Porretta
Analisi di preparazioni farmaceutiche - Analisi quantitativa (volume primo)
CISU Editore, Roma

Douglas A. Skoog, Donald M. West
Fondamenti di chimica analitica
EdiSES, Napoli

David G. Watson
Analisi Farmaceutica - Terza edizione
Edra LSWR, Milano

Supporting material:
Avaialble in digital format by download from Ariel site.
Assessment methods and Criteria
The unit of Laboratory for Quantitative Analysis does not provide a written or oral exam, because it considered passed when the student has correctly carried out at least 50% of the analysis and obtained a positive evaluation on his operational capabilities and its autonomy in executing analytical methods. When the student passes this unit, he can access to the examination of the unit of Principles of Quantitative Pharmaceutical Analysis, which includes a written test with 6 questions, for a total of 24 points, that must be completed in 2 hours. The remaining 6 points derive from the evaluation of the activity carried out in the laboratory.
For the exam, it is necessary to download the tables from the Ariel Web site and have a calculator. The use of mobile phones instead of the calculator is NOT allowed.
Laboratory for quantitative analysis
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 2
Single bench laboratory practical: 32 hours
Principles of quantitative pharmaceutical analysis
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 6
Lessons: 48 hours