87597 - Analysis of Medicines I

Learning outcomes

At the end of the course, which also includes laboratory practice, the student:

- acquires the theoretical and practical knowledge for the implementation of weighing, handling and transfer solid and liquid samples, and for the preparation of related solutions, and is able to critically evaluate the experimental data obtained for qualitative analysis according to the European Pharmacopoeia;

-acquires the theoretical and practical knowledge for the identification and quality control of inorganic compounds of pharmaceutical interest, through specific chemical tests and basic analytical methods reported by the Italian Official Pharmacopoeia and the European Pharmacopoeia.

Course contents

Module 1 - Inorganic qualitative analysis I

Lessons

Introduction: Aim of the course. Inorganic drugs. The European Pharmacopoeia (Eur. Ph.) and the Italian Official Pharmacopoeia (F.U.).

Solubility of inorganic salts: solubility product and modification of chemical equilibrium for analytical purposes. Formation and dissolution of precipitates. Complex ions formation.

Introduction to qualitative pharmaceutical analysis: bases of colour theory. Reactions useful for qualitative analysis of cations: precipitation of sulphides, precipitation of amphoteric hydroxides, formation of complex ions and their salts. Analysis of mixtures of salts in pharmaceutical formulations.

Identification of inorganic drugs following Eur. Ph. Cations: biologically active compounds and reactions useful for the identification of silver, mercury, copper, bismuth, aluminum, iron, zinc, calcium, barium, magnesium, lithium, sodium, potassium, ammonium ion. Introduction to atomic emission spectroscopy for the identification of cations. Anions: biologically active compounds and reactions useful for the identification of acetates, chlorides, bromides, iodides, carbonates and bicarbonates, nitrates, sulphates, phosphates.

Introduction to quality control of drugs: limit tests.

Laboratory practice

In the laboratory practice sessions, the techniques acquired in the academic lessons will be applied to the qualitative analysis of drugs and pharmaceutic formulations:

- identification reactions of cations and anions of pharmaceutical interest following Eur. Ph.

- identification of unknown inorganic drugs following Eur. Ph.

- identification of inorganic drugs in pharmaceutical formulations.

 

Module 2 - Inorganic qualitative analysis II

Lessons

Sampling of inorganic substances of pharmaceutical interest: fundamentals and critical issues of the sampling phase of inorganic compounds in solid and liquid form. Weighing techniques on balances of different types, for substances in solid form and for substances in liquid form. Types of containers for the sampling of inorganic salts of pharmaceutical interest.

Storage of salts and related solutions: instability issues (e.g. identification of deliquescent compounds), storage conditions and types of storage containers.

Solubility of inorganic salts: solubility tests in water and in the main organic solvents, according to the European Pharmacopoeia.

Preparation of solutions: solubilization and mixing of active ingredients of pharmaceutical interest according to the European Pharmacopoeia. Filtration procedures. Potentiometric pH measurement of aqueous solutions: preparation of S solutions and buffer solutions according to the European Pharmacopoeia and pH measurement using different acquisition methods.

Elaboration and evaluation of analytical data: elaboration of experimental data according to the main international guidelines. Comparative and critical evaluation of the experimental results and of the performances of the used analytical methods.

Laboratory practice

During the laboratory practice, the knowledge acquired during the theoretical lessons will be experimentally exploited, in order to carry out an effective qualitative analysis of the main inorganic compounds which constitute some of the most known drugs currently in use:

- Different types of weighing of inorganic salts

- Solubility tests in water and in the main organic solvents for analysis

- Identification of deliquescent substances and related problems of handling and storage

- Preparation of buffer solutions and S solutions according to the European Pharmacopoeia

- Potentiometric pH measurement.

Readings/Bibliography

Teaching material for lessons and laboratory is available for students at the dedicated Unibo website. For further reading, the following books are suggested:

1. V. Cavrini, V. Andrisano, Principi di Analisi Farmaceutica. Società Editrice Esculapio, Bologna.

2. European Pharmacopoeia

3. G. Caliendo, Manuale di analisi qualitativa. Edises (2019)

4. A. Carta. M.G. Mamolo, F. Novelli, S. Piras, Analisi Farmaceutica Qualitativa. Edises (2011).

Teaching methods

As regards the teaching methods of this course unit, all students (including all the international incoming exchange students, i.e. ERASMUS) must attend Module 1, 2 [https://www.unibo.it/en/services-and-opportunities/health-and-assistance/health-and-safety/online-course-on-health-and-safety-in-study-and-internship-areas] of health and safety course online, while Module 3 is to be attended in class. Information about Module 3 attendance schedule is available on the website of your degree programme ("studiare"--"formazione obbligatoria su sicurezza e salute").

The course includes lessons and laboratory practice, both with mandatory attendance. It is divided in two didactic modules:
- Inorganic qualitative analysis I, 3.5 ECTS (1.5 ECTS of lessons e 2 ECTS of laboratory practice)
- Inorganic qualitative analysis II, 2.5 ECTS (1.5 ECTS of lessons e 1 ECTS of laboratory practice).

Both modules include laboratory activity that will allow every single student to carry out analyses concerning the subjects of both of them. To allow for the best fruition of the laboratory, students will be divided into groups, attending laboratory practice sequentially.

The lessons are intended to provide basic knowledge of the chemical methods of European Pharmacopoeia and Italian Official Pharmacopoeia applied to the analysis of inorganic drugs and their formulations, as well as the main methods for sampling inorganic salts and preparation of their solutions.

The laboratory practice is carried out individually by each student under the supervision of the teacher and the tutors. The students are led to apply the methods described in the European Pharmacopoeia and the Italian Official Pharmacopoeia for a reliable preparation of solutions and mixtures, for the identification of inorganic drugs and their formulations.

Assessment methods

The final examination will evaluate the achievement of the following skills:

- Know and know how to practically carry out the identification reactions of active ingredients of inorganic drugs.
- Know the methods reported in the European Pharmacopoeia for quality control of drugs (limit tests).
- Know mechanisms of action and toxicity of inorganic drugs.
- Acquire good knowledge on qualitative analysis terminology.
- Acquire the theoretical fundamentals and practical skills related to inorganic salts and preparation of their solutions.
- Achieve the ability to process and critically evaluate experimental analytical data.
- Prove to have the ability to integrate the concepts acquired in the course with those of previous years and to be able to address the courses of the following years.

At the end of the laboratory practice of each module, the student will carry out a practical test consisting in the application of the methods reported in the European Pharmacopoeia to identify two inorganic drugs (module 1) and in the identification of inorganic salts by preparing the related solutions according to the European Pharmacopoeia (module 2). These tests will not be given a mark, but the results will be taken into account for the final grade, together with the whole laboratory work. Taking the practical tests, which will be always valid with no time limitation, is compulsory for the oral exam.

These practical tests will be followed by an oral examination for each module. The outcome of this examination is considered valid for the final assessment if both of them are taken in the same exam session. During the examination, the student will be asked questions on subjects dealt with during the course, in order to assess the acquisition of the expected skills, and includes reading and discussion of some of the monographs of the European Pharmacopoeia. The student should be confident in the knowledge acquired from previous courses, in particular inorganic chemistry. The final grade derives from the evaluation of the marks obtained in both modules and is integrated with the results obtained in the practical tests scheduled at the end of the laboratory.

Students should make an online appointment for the exam using the AlmaEsami platform. Dates are appointed in dedicated periods for all students, and for students registered over the 5th year other appointments can be made with the teachers throughout the year.

Students with a validated signature of attendance, acquired in their previous career, should take the practical test before taking the oral exam.

 

Teaching tools

Lessons will be held by using common audio-visual media. The laboratory practice will be carried out individually by each student in didactic laboratories especially equipped with chemical reagents and analytical instrumentation necessary for drug analysis.

Links to further information

https://www.unibo.it/sitoweb/silvia.gobbi

Office hours

See the website of Silvia Gobbi

See the website of Laura Mercolini