11438 - Drug Analysis II (GR.B)

Learning outcomes

At the end of the course, which will include laboratory experiments in a single place, the student will possess knowledge of methods of quantitative analysis, volumetric and instrumental, reported in the monographs of the European Pharmacopoeia (Ph. Eur) and the Italian Official Pharmacopoeia (F.U.I.) for the determination of the purity of active ingredients and the content of drugs in commercial formulations. In particular, the student is able to: - applythe knowledge to real problems (quantitative analysis and quality control of pharmaceutical preparations) - propose alternative methods of analysis, rationally justifying the choices made on the basis of the know how.

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, new edition 2011 (in press).

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. 32nd, United States Pharmacopeial Convention, 2009.

2) European Pharmacopoeia, Ed. 7th, 2011.

3) Farmacopea Italiana, Ed. XII, 2009.

4) Index Merck, Ed. 14th, 2006.

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 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.

For the oral examination, registration is required through the list of AlmaEsami . The students, of which the Council validates the signature offrequency acquired in previous career, must pass the laboratory practice test before the oral exam.

Teaching tools

Photocopies of lesson slides and of papers on drug analysis, provided by the teacher.

The students can use one of the Analytical Chemistry textbooks they already possess.

Italian, European and United States Pharmecopoeias are available for reference.

Office hours

See the website of Maria Augusta Raggi