90965 - Drug Analysis I (GR.A)

Course Unit Page

SDGs

This teaching activity contributes to the achievement of the Sustainable Development Goals of the UN 2030 Agenda.

Good health and well-being Quality education

Academic Year 2021/2022

Learning outcomes

After attending the lessons and undergoing the examination of the Drug Analysis I course, students: - know some volumetric and instrumental techniques of quantitative analysis included in European Pharmacopoeia (Ph. Eur.) and Farmacopea Ufficiale Italiana (F.U.I.) monographies for the determination of active ingredient and other raw material purity, as related to their use in the preparation of pharmaceutical formulations; - know how to apply these analytical techniques for the determination of the active ingredient content in pharmaceutical formulations; - are able to implement the methods they learned to real world problems (quantitative analysis of known compounds) and to novel problems in the quantitative drug analysis field; - can communicate and discuss the knowledge they possess in the field of volumetric and instrumental drug analysis; - can autonomously study and delve into the course topics.

Course contents

MODULE 1 - DRUG ANALYSIS I THEORY

Teacher: Professor Roberto Mandrioli

 

Introduction.
Aim of the course. Introduction to quantitative analysis. The Italian Official Pharmacopoeia (F.U.) and the European Pharmacopoeia (E.P.). Safety in the laboratory environment.
Introduction to drug analysis.
Introduction to volumetric analysis. Glassware and its use. Electronic balances. Concentration units. Normality, equivalents, calculus in volumetric analysis. Standard solutions. Primary standards, their properties and use.

Quantitative analysis
Neutralisation titrations. Titration curves of acid and bases. Polyprotic acids. Neutralisation indicators. Acidic and basic titrants. Primary standards for acidimetry and for alkalimetry.  Examples of acid-base titrations according to Eur. Ph.
Precipitation titrations. Precipitation titration curves. Common precipitation indicators and their use. Standard solutions used in precipitation titrations. Determination of halides by Mohr's, Volhard's and Fajans' methods. Practical aspects, limitations and applicability of the methods. Examples of precipitation titrations according to Eur. Ph.
Redox titrations. Introduction and theoretical aspects. Standard reduction potentials and the SRP list. Redox titration curves. Factors influencing the shape and position of redox titration curves. Redox indicators and specific indicators. Permanganometry. Properties, reactions and use of permanganate solutions. Identification of the final point. Standardisation of permanganate solutions. Examples of permanganometric titrations according to Eur. Ph. Iodimetry. Preparation and use of iodine solutions. Standardisation of iodine solutions. Examples of iodimetric titrations according to Eur. Ph. Iodometry. Principles, applications, properties. Use of starch water as an indicator. Standardisation of thiosulphate solutions. Examples of iodometric titrations according to Eur. Ph. Cerimetry. Properties and preparation of Ce4+ solutions. Standardisation of Ce4+ solutions. Examples of cerimetric titrations according to Eur. Ph.
Chelometric titrations. Complex formation and instability constants. Complexometric titration curves. Titrations employing EDTA. Conditional formation constant, alpha and their relationship to pH. Indicators for EDTA titrations. Standardisation of EDTA solutions. Direct titrations, back-titrations, displacement titrations, titrations based on indicators for an added metal ion, indirect titrations. Masking agents, masking and demasking. Analysis of complex cations mixtures. Water hardness. Examples of complexometric titrations according to Eur. Ph.
Conductimetry. Theory: electrical conductivity of electrolytic solutions. Conductance cell. Specific conductivity and equivalent conductivity. Conductimetric titration curves. Conductimetric titration techniques.
Ultraviolet and visible spectrophotometry. Keypoints. Factors governing absorption of radiation in the UV/vis region. Beer-Lambert law. Instrumentation. Calibration curves and how to build them. Choice of the optimal wavelength for analysis. UV spectra of some representative drugs. Applications in pharmaceutical analysis.


 

MODULE 2 - DRUG ANALYSIS I LABORATORY

Teacher:Professor Roberto Mandrioli

 

Standardization of NaOH with potassium phthalate. 

Standardization of HCl with Na2CO3 and NaOH. Purity of acidic compounds according to E.P.
Standardization of AgNO3. Purity of NaCl.
Standardization of Na2S2O3 and of KMnO4. Purity of redox compounds according to F.U.
Standardization of EDTA. Purity of ZnO. Water hardness.
The unknown concentration of inorganic ion solutions will be determined during the lab course.

Conductimetric titration of sodium acetate, acetylsalicylic acid.
Calibration of absorbance scale by using a cyanocobalamine solution (calibration graph), spectrophotometic determination of cyanocobalamine Spectrophotometric determination of the acetaminophen content in a tablet formulation.

Readings/Bibliography

A. Carrieri (Ed.)
Manuale di Analisi Quantitativa dei Medicinali
EDISES, Napoli, 2019
ISBN: 978-88-3319-044-0

G.C. Porretta
Analisi di preparazioni farmaceutiche - Analisi quantitativa
CISU, Roma, 2011
ISBN: 978-88-7975-529-0

Teaching methods

The course takes place during the second semester and is divided into two parts, 40 hours (5 ECTS Credits) of lessons and 45 hours (3 ECTS Credits) of laboratory practice; attendance is mandatory.
Volumetric analysis is explained and applied through laboratory experiments for the purpose of drug purity controls and inorganic active principle determinations.

Laboratory practical is carried out individually, with a final test.

Considering the activities and teaching methods adopted in this course, attending it requires the students to have already completed modules 1 and 2 (in e-learning mode at this web address) as well as module 3 (in person) of the specific "Health and Safety in places of study" course. An updated schedule and the manner of attending module 3 are available in the corresponding section of the Graduation Programme webpage.

Assessment methods

The examination includes an oral examination concerning both parts of the course, aiming to verify the knowledge acquired as stated by the learning outcomes. This examination, which could also include the reading and discussion of some of the monographs of the European Pharmacopoeia and F.U.I., shall be considered positive on the basis of correct answers to questions related to topics covered during the course.
Since the course includes practical exercises regarding the determinations described in the European Pharmacopoeia and F.U.I., the results obtained in such exercises will contribute to the definition of the final grade.

Teaching tools

The theoretical lessons will be held by using common audio-visual means.
Practical activities will be carried out in laboratories equipped with all necessary chemical reagents and analytical instrumentations.

Office hours

See the website of Roberto Mandrioli