11438 - Drug Analysis II (B)

Learning outcomes

The course has the aim of forming professionals in the field of quantitative pharmaceutical analysis. This is achieved by the practical application of basic notions of analytical chemistry. By learning and applying different analytical methodologies, the student acquires the competence, the experience and the manual ability needed to correctly deal with different analytical problems, such as the detemination of an active principle content, or of its purity, or the quality control of commerical formulations. The course also provides basic knowledge of behaviour rules and safety regulations during laboratory work.

Course contents

INTRODUCTION: Importance of chemical analysis in the pharmaceutical field. Analytical method classification and working ranges. How to express concentration measures.

VOLUMETRIC ANALYSIS: Basic principles. Reactions and reagents in volumetric analysis. Primary and secondary standards. Calculations. Precipitation titrations: Titration curves, factors which influence the evidence of the final point. Indicators. Titrating solutions and their standardisation. Mohr, Volhard and Fajans titrations. Application: analysis of halides. Acid-base titrations: Titration curves of strong acids andstrong bases.. Indicator theory. Titration curves of weak acids and weak bases. Titration curves of polyprotic acids. Analysis of different organic and inorganic acids.  Nonaqueous acid-base titrations: Titration curves and inidcators in the nonaqueous environment. Quantitative analysis of drugs according to Italian and European Pharmacopeias. Complexometric titrations: Inorganic complexing agents, polycarboxylic acids. EDTA: complexes, titration techniques, conditional formation constant, titration curves. Metallochromic indicators. Quantitative complexometric analysis. Redox titrations: Oxidising and reducing agents. Nernst equation. Standard and formal electrodic potentials. Redox titration curves. Indicators. Calculation of equilibrium constant and potential at the endpoint. Permanganometry, cerimetry, iodimetry, iodometry, bromometry.

ELECTROCHEMICAL ANALYSIS: General principles and classifications. Potentiometric methods:. Glass electrodes and pH measurement. Potentiometric, biamperometric and bipotentiometric titrations. Water determination with Kar Fischer method.  Voltammetric methods: Polarography. Ilkovic equation. Conductometric methods: Conductivity measurement. Conductometric titrations of acids, bases, salts..

SPECTROSCOPIC ANALYSIS: Absorption and emission. UV-Visible absorption spectroscopy: Absorption spectra. Lambert-Beer's law. Instrumentation. Quantitative analysis of active principles in formulations. Mixture analysis. Molecular fluorescence spectroscopy: Emission spectra. Emission intensity. Quenching. Spectrofluorimetric analysis of drugs.

SEPARATION TECHNIQUES: Fundamentals of chromatography; HPLC. Basis and modes of capillary electrophoresis (CE). Application of HPLC and CE to drug analysis.

 

LABORATORY PRACTICE

Acid-base titrations. Potentiometric and conductometric titrations. Precipitation titrations. Nonaqueous acid-base titrations. Redox titrations. Complexometric titrations. Spectrophotometric and spectrofluorimetric analysis. Quality control of pharmaceutical formulations.

Readings/Bibliography

 Non-mandatory Textbooks

1) PORRETTA, Analisi di preparazioni farmaceutiche, Ed. CISU, 2000.

2) RUBINSON, RUBINSON, Chimica analitica strumentale, Ed. Zanichelli, 2002.

3) HARRIS, Chimica analitica quantitativa, Ed. Zanichelli, 2005.

4) SKOOG, WEST, Chimica analitica, Ed. SES, 1987  

 

Reference Textbooks

1) United States Pharmacopoeia, Ed. 28°, United States Pharmacopeial Convention, 2005.

2) European Pharmacopoeia, Ed. 6th, 2008.

3) Farmacopea Italiana, Ed. XII , 2009.

4) Index Merck

5) WATSON, Analisi farmaceutica, Ed. EdiSES, 2003

Teaching methods

The course is divided into 40 hours of theoretical lessons and 48 hours of laboratory practice. Attendance is mandatory.

Laboratory practice: explanation and application of volumetric and instrumental analysis for the purity control of drugs and for the quantitation of active principles in commercial formulations.

Assessment methods

Oral examination, which can only be taken after the laboratory practice.

A final practical examination is carried out at the end of the laboratory practice. Its outcome is part of the overall evaluation.

Teaching tools

Lesson notes, papers provided by the teacher on drug analysis.

Italian, European and United States Pharmecopeias are available for consultation.

Office hours

See the website of Maria Augusta Raggi