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 identification and quality control of inorganic compounds of pharmaceutical interest, through specific chemical tests and analytical techniques. He is able to apply the knowledge acquired for the use of methods reported by the Italian Official Pharmacopoeia and the European Pharmacopoeia.

Course contents

Module 1 - Inorganic qualitative analysis I

Introduction to qualitative pharmaceutical analysis. Aim of the course. Introduction to qualitative analysis. 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. Formation and dissolution of precipitates.

Identification of inorganic drugs.

Cations. Biological roles, toxicological aspects, biologically active compounds and reactions used to identify silver, lead, mercury, antimony, bismuth and copper. Characteristics and differences in the precipitation of sulphides Characteristics of hydroxydes: anphoter hydroxydes. Biological roles, toxicological aspects, biologically active compounds and reactions used to identify aluminum, iron, zinc, manganese, calcium, barium, magnesium, sodium, lithium and potassium. Ammonium ion. Systematic analysis of cations.

Principles of color theory. Introduction to atomic emission spectroscopy: flame test for the identification of cations.

Anions. Biological roles, biologically active compounds and reactions used to identify acetates, borates, chlorides, bromides, iodides, carbonates and bicarbonates, nitrates, sulphates, phosphates, sulphides and thiosulphates, oxalates. Hydrogen peroxide.

Introduction to complex ions.

Semi-quantitative analysis of inorganic impurities in drugs: limit tests.

Module 2 - Inorganic qualitative analysis II

Sampling of inorganic substances of pharmaceutical and toxicological interest: fundamental principles and critical points of the sampling phase of inorganic compounds in solid and liquid form. Weighing techniques on balances of different types, both for substances in solid form and for substances in liquid form.

Solution preparation: solubilization and mixing of active ingredients of pharmaceutical interest according to the European Pharmacopoeia. Preparation of buffer solutions and pH measurement.

Sample pretreatment: fundamentals and application of methods for sample preparation and treatment with the purpose of separating the analytes from excipients. Comparison among filtration techniques, solid-liquid extraction (S/L) and liquid-liquid extraction (L/L).

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

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)

Teaching methods

As regards the teaching methods of this course unit, all students must attend Module 1, 2 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

The course includes lessons and laboratory practice, both with mandatory attendance. It is divided in two didactic modules:
- Inorganic qualitative analysis I, 4 ECTS (2 ECTS of lessons e 2 ECTS of laboratory practice)
- Inorganic qualitative analysis II, 3 ECTS (2 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 and instrumental pharmacopoeial methods applied to inorganic drug identification, as well as the main methods for sampling, preparation and treatment of solid and liquid samples.

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 Pharmacopoeia to confirm the identity of inorganic drugs and the procedures to use for a reliable preparation of solutions and mixtures.

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 and know how to practically carry out the pharmacopoeial methods 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 sampling, preparation and treatment of solid and liquid samples.
- 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 should sit for a practical test consisting in the application of the pharmacopoeial methods to identify two inorganic drugs (module 1) and in the preparation of a solution according to the 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