11438 - Drug Analysis II

Course Unit Page

SDGs

This teaching activity contributes to the achievement of the Sustainable Development Goals of the UN 2030 Agenda.

Good health and well-being

Academic Year 2022/2023

Learning outcomes

The aim of the course including laboratory activity is to provide the theoretical and practical knowledge about the analytical procedures for the identification of inorganic and organic drug-related compounds, by means of chemical reactions and instrumental methods. Particular attention will be paid to the different methods reported in the European Pharmacopoeia or Italian FU.

Course contents

Introduction: Programme and aim of the course. The European Pharmacopoeia.

Module 1-Drug Analysis:

Characters. Intermolecular binding forces and physical state, colour.

Solubility. Solubility of inorganic salts, solubility product and modification of chemical equilibrium. Dissolution process of organic compounds, solvent properties (polarity and dielectric constant). Solutes: relationship between chemical structure and solubility. Solubility test.

Chemical analysis of drugs. Elemental analysis: heating test and Lassaigne’s test. Analysis of inorganic drugs: reactions for the identification of cations (silver, mercury, bismuth, copper, aluminium, iron, zinc, calcium, barium, magnesium, sodium, lithium, potassium, ammonium) e anions (chloride, bromide, iodide, acetate, sulfate, phosphate, carbonate and hydrogen carbonate, nitrate). Flame test. Identification reactions of functional groups of organic drugs: unsaturated carbons, aromatics, alcohols, phenols, aldehydes and ketones, acids and esters, amines.

Module 2-Instrumental Methods:

Determination of physical properties. Melting point, boiling point, density, refractive index, optical rotation.

Absorption spectroscopy: Principles and apparatus of Infrared spectroscopy and Nuclear Magnetic Resonance spectroscopy and applications to the identification of drug.

Extraction techniques: liquid-solid extraction, liquid-liquid extraction (partition coefficient, effect of pH and salts).

Chromatographic techniques: The chromatographic process, separation mechanisms (adsorption, partition, ion exchange, molecular exclusion, affinity). Column and thin-layer chromatography (TLC).

Readings/Bibliography

Teaching material for lessons and laboratory is available for students at the website https://iol.unibo.it. 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 - P. Barbetti, M.G. Quaglia, L'Analisi qualitativa in chimica farmaceutica e tossicologica inorganica. Galeno Editrice.

Teaching methods

The course includes theoretical lessons and laboratory practice and attendance is mandatory for both. It is divided in two modules and includes 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 two groups doing laboratory practice sequentially.

The lessons are intended to provide the basic knowledge of the chemical and instrumental pharmacopoeial methods applied in drug identification.

The laboratory practice is carried out individually by the students under the supervision of the teacher and the tutor. The students are led to apply the methods described in the Pharmacopoeia to confirm the identity of drug and excipients. All the experiments are recorded by the student on a laboratory book and the obtained results are discussed with the teacher.

Assessment methods

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

- Know how to apply in practice the identification reactions of the active ingredients of inorganic, organo-metallic and organic drugs.
- Know the main analytical instrumental techniques for drug recognition and know how to apply in practice the techniques concerning IR, NMR, polarimetry, melting point and TLC.
- Prove 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, the student should sit for a test consisting in the application of the pharmacopoeial methods to identify two drugs and in writing a report for each of them. This test 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 test, which will be always valid with no time limitation, is compulsory for the oral exam.

This practical test will be followed by an oral examination for both modules to be taken with the two teachers, in which 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 with the knowledge acquired from previous courses, in particular inorganic and organic chemistry. The final mark for the exam will also take into account the results of the practical test.

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

Teaching tools

Lessons will be held by using slides. The laboratory practice will be carried out individually by each student in laboratories equipped with chemical reagents and analytical instrumentation.

Links to further information

https://www.unibo.it/sitoweb/anna.minarini/

Office hours

See the website of Anna Minarini

See the website of Silvia Gobbi