LABORATORY OF DRUG ANALYSIS I A - L

The purpose of this module is to introduce the student to the principal inorganic compounds of the pharmaceutical interest and to the chemical behavior of cations and anions present in them; with this knowledge, the student will understand the analytical aspects related to the use of these substances as well as their pharmaceutical and toxicological use.
At the end of this module the student will be able to apply the knowledge acquired to analyze inorganic compounds either alone or in mixture in order to recognize the presence and determine their purity; for example, given a sample constituted by a mixture of inorganic compounds, the student will be able to perform the proper sequence of reactions for the analytical separation and identification of the ions therein. He will also be able to understand the identification reactions of some inorganic ions reported in the Italian and European Pharmacopoeia.

TEACHING METHODS
Theoretical lessons and laboratory practice. Overall workload: 200 (h): Lectures: 42, Practical laboratory: 36, Individual study: 122.
ASSESSMENT METHODS
Reports on laboratory activities, laboratory proof, and oral examination.

The teacher uses three different teaching methods:

1. exhibition method: the lesson;

2. active method: the use of procedures that actively involve the student in the learning process;

3. operative method: laboratory activity with single and group experiments, manual and instrumental.

IN CLASSROOM (4.5 credits)

MODULE 1 (1.5CFU): GENERAL INFORMATION ABOUT OPERATIONS AND LABORATORY TECHNIQUES.
• Overview of analytical methods (classification, different stages of analysis, applications). Content of Italian Official Pharmacopoeia (FUI) and European Pharmacopoeia.
• Chemical reactions. Balancing of chemical equations, classification of chemical reactions
• Formation of precipitates- Complex formation.
• Equipment and instruments in the laboratory.
• Technical and basic operations in the semi-micro analysis. Standard operation procedures for sample pretreatment: dissolution, precipitation, filtration, centrifugation, decantation, pH measurement.
• Safety in the laboratory. Safety standards and behavior, classes and hazard symbols of harmful substances, safety data sheets, personal protective equipment, accident prevention, waste disposal, first aid items.
• Good practice in the laboratory.
• Introduction to chromatographic methods. Overview, classification, mechanisms and separation techniques. Variables, equations, and basic parameters. Stationary phases and mobile phases. Operational techniques. TLC.

PURPOSES AND PRODUCTS OF LEARNING (LEARNING OUTCOMES) - MODULE 1
The purpose of this module is to familiarize students with the various types of analysis, operations, and techniques in the pharmaceutical field. The student will be able to deal with analytical problems from theoretical and practical point of view; he will then properly approach an analysis using the most appropriate technique, measure, and operation; he will also be able to make some simple, both manuals and instrumental, laboratory operations and he will be able to put into practice the behavioral and safety rules necessary for such kind of analysis.
MODULE 2 (3CFU): INORGANIC SUBSTANCES OF PHARMACEUTICAL AND TOXICOLOGICAL INTEREST REPORTED IN THE FUI AND/OR IN THE EUROPEAN PHARMACOPOEIA.
Properties, chemical characters, analytical and identification reactions, and pharmaceutical properties of the following ions (in the dry sample): carbonates, sulfites, acetates, borates, ammonium ion.
Properties, chemical characters, analytical and identification reactions, and pharmaceutical properties of the following cations (in solution sample, with particular reference to the underlined elements):
silver, mercury (I), lead;
arsenic, antimony, tin, mercury (II), lead, bismuth, copper, cadmium;
aluminum, iron, zinc, manganese, cobalt, nickel, chromium;
calcium, barium, strontium, magnesium;
sodium, lithium, potassium.
Properties, chemical characters, analytical and identification reactions, and pharmaceutical properties of the following anions (in solution sample): halides, oxalates, phosphates, sulfates, nitrates.
Case studies.

LABORATORY EXERCISES (1.5 credits)
Module 1:
Laboratory safety rules. Simple procedures of sample pretreatment: dissolution, precipitation, filtration, centrifugation, measurement of PH. Analysis of simple mixtures by means of thin-layer chromatography (TLC).
Module 2:
Analysis of cationic and anionic species:
analysis performed directly on the dry samples:
• carbonates, acetates, borates, ammonium ion.
analysis performed on a solution sample:
• analysis of cations (alone and/or in mixture): Ag⁺, Al³⁺, Fe²⁺ / Fe³⁺, Ca²⁺, Mg²⁺.
• analysis of anions (alone and/or in a mixture): Cl^-, Br^-, I^-, C₂O₄^2-, PO4^3-, SO₄^2-, NO^3-.

• identification of cations and/or anions in an unknown mixture.

D. A. Skoog, F.J. Holler, S. R. Crouch, Chimica analitica strumentale, Edises

R.L Snyder, J.J. Kirkland, J.L. Giajch, Practical HPLC method development,

Wiley; C. F. Poole, The essence of chromatography, Elsevier.

T. R. Hogness, W. C. Johnson, A. R. Armstrong, Analisi qualitativa ed equilibrio chimico, Piccin;

A. Araneo Chimica analitica qualitativa, Ambrosiana;

P. Barbetti, M. G. Quaglia, L’analisi qualitativa in chimica farmaceutica e tossicologica inorganica. Vol. 1, Galeno;

Farmacopea Ufficiale Italiana XI edizione.

EUROPEAN PHARMACOPOEIA

Selected articles and reviews on specific arguments.

Lecture slides, analytical laboratory guideline, and methods (see "STUDIUM").