OVERVIEW

The course deals with (i) the pre-treatment of complex matrices containing bioactive compounds, (ii) and the quantitative determination of substances of pharmaceutical interest. It is developed with theoretical and practical lessons. The theoretical ones are preliminary to the practical ones and to the whole course comprehension. The main topics of the course are listed as follows.

AIMS AND CONTENT

LEARNING OUTCOMES

The course deals with the pre-treatment, extractive techniques and purification methods of bioactive molecules and substances of pharmaceutical interest. Instrumental and classical quantitative determination methods will be deepened, such as titration analysis. This course is developed with theoretical and practical lessons.

AIMS AND LEARNING OUTCOMES

The course allows to acquire theoretical and practical information regarding the main methods of sample pretreatment and purification. These methods include chromatography and instrumental analysis such as gas chromatography and HPLC. Specific theoretical and practical information will be acquired in terms of quantitative analysis of bioactive compounds, such as volumetric analysis, in particular in the areas of acidimetric and alkalimetric titrations, complexometric, redox and precipitation titrations. The laboratory activities concern sample pre-treatment and purification techniques and the dosage of drugs. At the end of the course, the student will be able to set up discontinuous separations by identifying the acid-basic behavior and the polarity of the components of the mixture to be studied, to analyze and discuss the extraction and chromatographic separation procedure. The student will be able to identify the most suitable titration methods, given a compound of pharmaceutical interest and apply titration techniques such as acidimetric and alkalimetric titrations, complexometric, and redox titrations.

PREREQUISITES

Inorganic chemistry.

TEACHING METHODS

The course is developed with theoretical and practical lessons (96 hours). The course is divided into theoretical lessons, covering the topics of the program dedicated to the techniques of purification of the sample and quantitative analysis of the same. The planned laboratory activities will be aimed both at techniques of treatment and purification of the sample through various extraction and/or chromatographic techniques, and at the quantitative dosage of drugs. During the course, exercises will be carried out to simulate the practical laboratory tests and for practice in the written exam.

Any Student with documented Specific Learning Disorders (SLD), or with any special needs, shall reach out to the Lecturer(s) and to the dedicated SLD Representative in the Department ( Prof. Luca Raiteri, Luca.Raiteri@unige.it ) before class begins, in order to liaise and arrange the specific learning methods and ensure proper achievement of the learning aims and outcomes. VERY IMPORTANT: any request for compensatory tools and adaptations in the exam MUST be done within 10 working days before the date of the exam according to the instructions that can be found at https://unige.it/disabilita-dsa/comunicazioni

SYLLABUS/CONTENT

• Theoretical topics

• Guidelines on laboratory safety and chemical use.
• Chemical properties of bioactive compounds, apparatus and laboratory instruments.
• Methods for sample purification: techniques of preparing sample: filtration, extraction, distillation.
• Sample characterization: melting point, boiling point and refractive index determination.
• Chromatography techniques, Gas chromatography and HPLC.
• Classification and selection of analitycal methods.
• Calculation used in pharmaceutical analysis. Sampling, standardization and calibration.
• Introduction to the quantitative determination of compounds registered in FU XII Ed. and FE VIII Ed.
• Introduction to volumetric titrations in pharmaceutical analysis: chemical
• Quantitative determination and applications: neutralization titrations, complexation and precipitation reactions and titrations, oxidation/reduction titrations, Diazotization Titration.
• Practical trainings simulations

• Practical trainings

  Extraction with solvent, distillation in vacuo. TLC.

  Chromatographyc separation and analysis of a mixture of drugs. Quantitative determination of drugs by mean of neutralization titrations, complexation and precipitation reactions and titrations, oxidation/reduction titrations.

RECOMMENDED READING/BIBLIOGRAPHY

• Principi di Analisi Farmaceutica, Quarta Edizione - V. Cavrini e V. Andrisano, ESCULAPIO
• Analisi Farmaceutica David G. Watson Edra 2014
• Fondamenti di chimica analitica di Skoog e West, Terza Edizione - F. James Holler e Stanley R. Crouch, EDISES – ISBN 9788879598651
• Analisi chimico farmaceutica - F. Savelli e O. Bruno - PICCIN

TEACHERS AND EXAM BOARD

LESSONS

LESSONS START

Second semester. Please see, EasyAcademy.

Class schedule

The timetable for this course is available here: Portale EasyAcademy

EXAMS

EXAM DESCRIPTION

Written prior to oral test. The first one is about mixture separation and quantitative determination of one proposed bioactive compound. The oral test will cover all the course main topics including both a discussion of the course contents and of the laboratory activities carried out. The practical laboratory part is subject to evaluation and contributes to the final grade for this course, together with the grade obtained with the oral exam.

ASSESSMENT METHODS

The examination includes one written test and the oral test together with the evaluation of the experimental ability achieved by the student while attending to practical trainings in laboratory. The written test will test the knowledge acquired in identifying extraction methods of proposed compounds, in mixtures, recognizing their acid-base character. At the same time, the ability to propose titration methods for an inorganic salt will be tested. During the oral test, the theoretical knowledge regarding all the contents of the course, the skills acquired in discussing extraction and chromatographic separation methods of proposed mixtures, the skills in commenting on volumetric analysis techniques with respect to specific analytes, using appropriate technical-scientific language, will be assessed.