B2821 - Analysis of Drugs and Health Products II

Learning outcomes

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

-acquires the theoretical and practical knowledge about extraction and chromatographic techniques for purification and isolation of drugs

- knows and knows how to practically carry out the identification reactions and instrumental analytical methods reported in the European Pharmacopoeia and Italian FU for the analysis of drugs and other health products.

Course contents

Useful requirements for best approaching the learning experience: consolidated notions deriving from courses in previous years, with particular attention to inorganic and organic chemistry.

Module 1-Drug Analysis

European Pharmacopoeia and Italian FU. Monographs of substances of pharmaceutical interest.

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, proticity and dielectric constant). Solutes: relationship between chemical structure and solubility. Drugs solubility tests.

Chemical analysis of drugs. Qualitative elemental analysis.

Analysis of inorganic drugs: 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; biologically active compounds and reactions for the identification of cations (silver, mercury, copper, bismuth, aluminium, iron, zinc, calcium, barium, magnesium, lithium, sodium, potassium, ammonium) e anions (acetates, chlorides, bromides, iodides, carbonates and bicarbonates, nitrates, sulphates, phosphates). Elements of atomic emission spectroscopy.

Analysis of organic drugs: identification reactions of functional groups of organic compounds (unsaturated carbons, aromatics, alcohols, phenols, aldehydes, acids and derivatives, amines, xanthines).

Module 2-Instrumental Methods

Determination of physical properties. Boiling point: principles and applications. Boiling point determination. Distillation and vacuum distillation apparatus.

Melting point: principles and applications. Equipment for melting point determination. Melting point of solid mixtures.

Specific optical rotation. Polarimeter. Qualitative analysis of optically active compounds. Applications.

Refractive index. Refractometer. Principles and applications.

Absorption spectroscopy: Infrared (IR) spectroscopy: principles and applications, apparatus, interpretation of IR spectra for the identification of drugs.

Nuclear magnetic resonance (NMR) spectroscopy: principles and applications, apparatus, interpretation of proton NMR spectra.

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

Laboratory practice

The course includes laboratory practice aimed at applying the techniques acquired in both theoretical modules to the qualitative analysis of drugs and pharmaceutic formulations:

• identification reactions of cations and anions of pharmaceutical interest following Eur. Ph.
• Identification reactions of functional groups in organic compounds secondo Eur. Ph.
• drug solubility tests
• melting point determination
• polarimetric analysis of chiral substances
• IR spectroscopy
• thin-layer chromatography of pharmaceutical formulations
• identification of unknown drugs following Eur. Ph.
• identification of drugs in pharmaceutical formulations

Readings/Bibliography

Teaching materials for lectures and laboratory practice are available to students at the dedicated website. While these materials form the basis for studying the course, they should be supplemented with lecture notes and/or the recommended textbook. An adequate knowledge of the organization and structure of the European Pharmacopoeia is also required.

For further reading, the following book is suggested:

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

Teaching methods

The course includes theoretical lessons and laboratory practice. The attendance requirement is fulfilled by attending at least 80 % of laboratory sessions and 60 % of lectures. Attendance is recorded using the ‘Presenze studenti’ application.

The course (8 CFU) is divided in two theoretical modules (2.5 CFU, 20 hours each) and includes laboratory activity (3 CFU, 45 hours) 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 methods of Eur. Ph. 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, as pure substances or included in formulations. Students are required to record their daily lab work and the results obtained in a lab notebook. The notebook is reviewed by the teacher for any corrections and observations during the oral exam. Laboratory work is conducted with the assistance of lab technicians to ensure students are aware of the importance of working in compliance with safety regulations.

As concerns the teaching methods of this course unit, all students (including all the international incoming exchange students, i.e. ERASMUS) must attend Module 1, 2 online [https://www.unibo.it/it/servizi-e-opportunita/salute-e-assistenza/salute-e-sicurezza/sicurezza-e-salute-nei-luoghi-di-studio-e-tirocinio], while Module 3 on health and safety 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").

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, as pure substances or included in formulations.
- 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.

- Demonstrate to be confident in chemical and analytical-instrumental terminology.

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 monographs of the European Pharmacopoeia. The student should be confident with the knowledge acquired from previous courses, in particular inorganic and organic chemistry. Regarding learning assessment, the use of AI is prohibited. Any use constitutes a violation of academic integrity. The final grade is agreed upon by the teachers during the oral exam and also takes into account the results of the practical test, and the related written report, completed at the end of the laboratory practice.

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 teachers throughout the year using Almaesami.

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

Students with DSA or temporary or permanent disabilities are recommended to contact the competent University Office in advance (https://site.unibo.it/studenti-con-disabilita-e-dsa/en ). It will be the responsibility of the Office to propose any adaptations, which must however be submitted, at least 15 days in advance, to the approval of the teacher, who will evaluate them with respect to the educational objectives of the course.

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/silvia.gobbi

Office hours

See the website of Silvia Gobbi

See the website of Marina Naldi