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

Module 1-Instrumental Methods

Determination of physical properties.

Boiling point: principles and applications. Boiling point determination. Apparatus for distillation and vacuum distillation.

Melting point: principles and applications. Melting point determination equipment. Melting point of solid mixtures.

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

Refractive index. Refractometer. Principles and applications

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

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

Module 2-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).

The course includes laboratory practice aimed at applying the techniques acquired in both 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 material for lessons and laboratory is available for students at the dedicated 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

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 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. 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