The course, consisting in class lectures and lab practice, is intended to give knowledge of classic techniques for quantitative analysis and quality control of pharmaceuticals. During the course, students will acquire skills in the practical execution of quantitative analyses reported in pharmacopoeial monographs and in the interpretation of experimental data.
On successful completion of this course students will be able to:
Moreover, on successful completion of the lab practice, students will be able to:
Activities of the course are constituted by class lectures and case study along with laboratory experiences (single or group work). Attendance (at least 70%) at classes and laboratory experiences is mandatory. Attendance is attested by student’s own signature.
At the beginning of the course, laboratory shifts and the corresponding lab practice schedule are defined on the basis of the total student number.
During class lectures, all the subjects are presented in details. Students are asked to actively discuss about them and about a number of case studies.
During lab practice, students have to critically analyse experimental protocols and perform a number of quantitative analyses on samples of pharmaceutical interest. In lab, students are stimulated to discuss each other and with teachers about practical experiences and subjects seen during class.
At the end of every lab practice students have to write up and submit a report on the experience. The report is evaluated for the clarity of expression, correctness in the conduction of the analysis and the accuracy and precision of the final result. The report is given back to the student and commented on during the next lab session.
A trial is scheduled at the end of the lab practice.
Should teaching be carried out in mixed mode or remotely, it may be necessary to introduce changes with respect to previous statements, in line with the programme planned and outlined in the syllabus.
The final exam is oral.
To take the exam, students need to book on line at Portale studenti of Università di Catania webpage (www.unict.it). Booking list is opened about fifteen days before the exam date.
Learning assessment may also be carried out on line, should the conditions require it.
Generalities on chemical quantitative analysis
Materials, reagents and laboratory apparatuses. Laboratory safety. Validation of an analytical method. Accuracy and precision. Outlier tests: 4d test and Dixon’s test. Analytical balances, weighing operations and methods.
Volumetric analysis
Preparation of solution with known concentration; determination of the concentration of solutions. Volumetric glassware and calibration. Calculations in volumetric analysis.
Acid-base titrations
Acidimetric and alkalimetric titrations. Preparation and standardization of acid or basic solutions. Acid-base indicators. Neutralization titrations in non-aqueous solvents: generalities, intrinsic acidity and alkalinity, differentiating and leveling effects, solvent classifications. Equilibria in non-aqueous solvents, criteria for choosing a solvent.
Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia X ed. Determination of: Sodium Carbonate, Sodium Hydrogencarbonate, alkaline carbonates and hydroxides mixtures, alkaline carbonates and hydrogencarbonates mixtures, Ephedrine emihydrate, Nitrogen by Kjeldahl method, Ammonium salts, Tartaric acid, Phosphoric acid, Citric acid, Naproxen, Ibuprofen, Nimesulide, Omeprazole, Acetylsalicylic Acid, Benzyl Benzoate, Boric Acid, Saccharin, Nicotinamide, Diazepam, Aspartame, Atropine Sulphate, Sodium Benzoate, Morphine Hydrochloride, Sulfafurazole.
Precipitation titrations
Argentometric titrations. Preparation and standardization of a silver nitrate solution and of a ammonium thiocyanate solution. Titration methods (Mohr, Volhard, Fajans). Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia X ed. Determination of: Alkaline Halides, Chlorobutanol emihydrate.
Complexometric titrations
Titrations methods. Preparation and standardization of an EDTA solution. Complexometric indicators. Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia X ed. Determination of: Al, Bi, Ca, Mg, Pb, Zn, Hg, Fe salts. Determination of hardness in drinking water.
Oxidation-reduction titrations
Permanganometry, cerimetry, iodimetry, iodometry, bromometry.
Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia X ed. Determination of: Calcium salts, Ferrous salts, Hydrogen peroxide solution (3%) and expression of its concentration in volumes of oxygen; Ferrous sulphate Heptahydrate, Menadione, Paracetamol, Nifedipine; Sodium Sulphite Heptahydrate, Ascorbic Acid, Ascorbyl Palmitate, Captopril; Potassium Permanganate, Tosylchloramide Sodium, Hydrogen Peroxide, Ferric Chloride Hexahydrate; Isoniazid, Phenol.
Electroanalytical methods
Potentiometric determination pH. Potentiometric detection of the end-point in titrations. Biamperometric determination of primary aromatic nitrogen: applications to sulfamidics (Sulfadiazine) and Benzocaine described in Italian Pharmacopoeia XII ed. and European Pharmacopoeia X ed.
Spectroanalytical methods
UV-visible spectrophotometry
General discussion. Lambert-Beer law. Quantitative analysis: choice of the wavelength (l), general procedures for the quantitative determination. Linear regression analysis. Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia X ed. Determination of: Prednisolone acetate.
Fluorimetry
Principles and basic features of the technique, instrumentation, applications to the quantitative analysis of pharmaceutical substances.
The course includes lab practice. Lab practice schedule, for each academic year, is defined at the beginning of the course. A list of some typical laboratory experiences is the following:
Items 1 and 2 are textbooks, 3 -6 are reference books, Italian and European Pharmacopoeias (item 7) are the sources for ufficial quantitative analyses of pharmaceuticals