87602 - Drug Analysis III

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

Drug Solubility. Determination of solubility parameters. Type of solvents. Intermolecular forces: hydrogen bonding, Van der Waals and ionic interactions. Structure-solubility relationships. Solubility of weak acid and weak basic drugs.

Characterization of liquid drugs. Definition and determination of relative and absolute density. Definition and determination of refractive index. Abbe refractometer. Qualitative analysis of liquid drugs.

Characterization of solid drugs. Determination of melting point. Melting point variables.

Polarimetry. Specific optical rotatory power. Polarimeter scheme and polarimetric determination.

Spectroscopy techniques for the qualitative analysis of drugs:

(a) UV-VIS spectroscopy for the qualitative analysis of drugs in compliance with the Italian and European Pharmacopoeias. Scheme and use of double beams spectrophotometers.

(b) Infrared spectroscopy. Applications to drug analysis, identification of functional groups. Qualitative elemental analysis

Identification of drugs by chemical reactivity of functional groups. alkenes, alcohols, phenols, ketones, aldehydes, acids, esters, amines, amides, nitro-derivatives and sulfur compounds.

Identification of compounds inscribed in the Pharmacopoeia. Preliminary test: evaluation of the behavior of the substances when heated. Inorganic qualitative analysis. Qualitative elemental analysis: determination of the elements (C,N,O,S) of organic drugs by Lassaigne's test. Illustration of the systematic procedure for compound identification.

Extraction methods for sample pretreatment:

(a) Solid phase extraction (SPE): theory, type of sorbents, apparatus for SPE, matrices with different functionalities, RAM (restricted access matrices), molecularly imprinted polymers (MIPs). Extraction recovery; applications to pharmaceutical formulations.

(b) Solid phase microextraction (SPME): theory, apparatus for SPME, modus operandi, method optimization. Applications to pharmaceutical formulations.

LAB Tutorials:

Qualitative identification of drug substances by chemical and instrumental methods (spectrophotomer and IR spectometer, polarimeter, rifractometer).

Solid phase extraction (SPE) of ephedrine and sodium benzoate.

Readings/Bibliography

Readings/Bibliography

Teaching material for lessons and laboratory is available for students at the website http://iol.unibo.it.

For further reading, the following books are suggested:

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

European Pharmacopoeia and Farmacopea Ufficiale Italiana (current editions)

Teaching methods

The course includes lessons and laboratory practice and attendance is mandatory for both.

The lessons are intended to provide the basic knowledge of the chemical and instrumental pharmacopoeial methods applied in the 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 drugs and excipients. All the experiments are recorded by the student on a laboratory book and the obtained results are discussed with the teacher. The laboratory activity is carried out with the assistance of laboratory technicians in order to sensitize students to operate in compliance with safety rules.

Assessment methods

The learning assessment is established by means of laboratory practice test, to be carried out at the end of the lab activity, and final oral examination.
The lab practice test has to be passed before oral examination and  consists in the application of the pharmacopoeial methods to identify a drug and in writing a report . 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, it will be always valid with no time limitation and is compulsory for the oral exam.

The final grade will be established by evaluating the student performance on both lab activity and oral examination. The latter will consists in 3-4 questions on subjects dealt with during the course.

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.

Office hours

See the website of Alessandra Locatelli