ANALISI DEI FARMACI E DEI PRODOTTI PER LA SALUTE 1 - ANALISI DEI FARMACI E DEI PRODOTTI PER LA SALUTE 2 M - Z

Module ANALISI DEI FARMACI E DEI PRODOTTI PER LA SALUTE 2

The course aims to provide students with the theoretical knowledge and practical skills required for the quantitative analysis of pharmaceutical and health-related substances using volumetric and instrumental analytical techniques.

1. Knowledge and Understanding

Students will be able to describe and/or discuss:

• the fundamental principles of the different techniques used in quantitative pharmaceutical analysis;
• the main laboratory operations employed for the quantitative determination of active pharmaceutical substances;
• the analytical procedures reported in the Italian Official Pharmacopoeia and the European Pharmacopoeia.

Assessment methods: written examination questions and evaluation of practical laboratory activities.

2. Applying Knowledge and Understanding

Students will be able to apply:

• analytical procedures for the quantitative determination of various pharmaceutical active substances;
• the main laboratory techniques correctly and appropriately;
• volumetric and instrumental analytical methods for the determination of active substances.

Assessment methods: written examination questions and evaluation of practical laboratory activities.

3. Making Judgements

Students will be able to:

• critically analyze the experimental results obtained;
• assess the reliability of the analytical procedures adopted;
• interpret data derived from laboratory activities;
• identify possible sources of experimental error.

Assessment methods: evaluation of the experimental results obtained and practical laboratory activities.

4. Communication Skills

Students will be able to:

• describe the principles of quantitative analysis using appropriate scientific terminology;
• discuss the techniques adopted for the assay of active substances;
• accurately report experimental data.

Assessment methods: assessment of terminological accuracy and clarity of presentation in written examinations and laboratory reports.

5. Learning Skills

Students will be able to:

• independently deepen their understanding of the topics covered;
• retrieve information from up-to-date bibliographic sources;
• develop an autonomous study method useful for subsequent courses in pharmaceutical analysis.

The course consists of a total of 54 hours, divided into 31 hours (4.5 ECTS credits) of direct instruction (lectures) and 23 hours (1.5 ECTS credits) of interactive teaching (individual laboratory exercises/workstations in the lab). At the beginning of each academic year, a schedule of laboratory sessions is established and published, including:

1. Assignment of the workstation. Laboratory safety. Use of calibrated glassware and analytical balances.
2. Determination of the concentration of a NaOH solution. Use of acid-base indicators.
3. Standardization of an HCl solution using anhydrous Na₂CO₃ as a primary standard.
4. Quantitative determination of an unknown Na₂CO₃ sample by acidimetric titration.
5. Quantitative determination of an unknown sample of L-(+)-tartaric acid by alkalimetric titration.
6. Determination of total hardness in drinking water. Determination of mg/L of Ca²⁺ and Mg²⁺ ions.
7. Determination of the purity percentage of a caffeine sample using spectrophotometry. Application of the Beer-Lambert law.
8. Use and calibration of the pH meter. Potentiometric determination of the endpoint in an acid-base titration. Construction of the titration curve.
9. Quantitative determination of an unknown caffeine sample by spectrophotometry. Construction of the calibration curve.

If the course is delivered in blended or remote mode, appropriate adjustments may be made to the above, in order to ensure consistency with the syllabus.

According to the Academic Regulations (RDA), Article 12, University Educational Credits (CFU/ECTS), within the standard workload of 25 hours of total student commitment corresponding to one credit, the following may be included:

a) 7 hours devoted to lectures or equivalent teaching activities, with the remaining time dedicated to individual study;

b) at least 12 hours and no more than 15 hours devoted to classroom exercises or equivalent supervised activities (laboratories), with the remaining time dedicated to individual study and personal review.

The course consists of lectures and individual laboratory practical sessions. During the lectures, the theoretical aspects related to the quantitative analysis of substances of pharmaceutical and health interest will be discussed. The laboratory practical sessions will focus on the application of some of the analytical techniques covered during the lectures.

Attendance at both lectures and laboratory sessions is mandatory, as required by the academic regulations of the Degree Program in Pharmacy: https://www.dsf.unict.it/it/corsi/lm-13/regolamento-didattico.

Absences are permitted for no more than 30% of the total teaching hours, considering all forms of course activities. Attendance is compulsory. For laboratory practical sessions, students are strongly advised not to be absent except in unavoidable circumstances.

To participate in the practical laboratory sessions, it is MANDATORY to attend a training course on SAFETY IN TEACHING LABORATORIES, organized by University officials before the start of the practical activities.

Program (6 CFU)

Module 1 (3 CFU)

Introduction to Quantitative Chemical Analysis. Materials, reagents, and equipment used in the laboratory. Laboratory safety. Validation of an analytical method. Accuracy and precision. Rejection of outliers: the 4d method and Dixon’s test. Analytical balances, weighing operations, and weighing methods.

Volumetric Analysis

Preparation of standard solutions; verification and determination of solution concentration. Volumetric apparatus and calibration. Calculations in volumetric analysis.

Acid-Base Titrations

Acidimetry and alkalimetry. Preparation and standardization of acid and base solutions. Indicators. Acid-base titrations in non-aqueous solvents: general principles, intrinsic acidity and basicity, leveling and differentiating effects, classification of solvents. Equilibria in non-aqueous solvents and criteria for solvent selection.

Applications, with particular reference to the monographs reported in the 12th edition of the Italian Official Pharmacopoeia (FUI XII) and the 12th edition of the European Pharmacopoeia (Ph. Eur. XII) and their supplements. Determination of: sodium carbonate, sodium bicarbonate, mixtures of carbonates and alkaline hydrates, mixtures of alkaline carbonates and bicarbonates, ephedrine, amino nitrogen according to the Kjeldahl method, tartaric acid, phosphoric acid, citric acid, naproxen, ibuprofen, nimesulide, omeprazole, benzyl benzoate, acetylsalicylic acid, boric acid, saccharin, nicotinamide, diazepam, aspartame, sodium benzoate, and sulfafurazole.

Precipitation Titrations

Argentometry. Preparation and standardization of silver nitrate and ammonium thiocyanate solutions. Titration methods. Applications, with particular reference to monographs reported in the FUI XII and Ph. Eur. XII and supplements. Determination of: alkali halides and chlorobutanol.

Complexometric Titrations

Titration methods. Preparation and standardization of an EDTA solution. Applications, with particular reference to monographs reported in the FUI XII and Ph. Eur. XII and supplements. Determination of salts of Al, Ca, Mg, Pb, Zn, Hg, and Fe. Determination of water hardness.

Redox Titrations

Permanganometry, cerimetry, iodimetry, iodometry, and bromometry.

Applications, with particular reference to monographs reported in the FUI XII and Ph. Eur. XII and supplements. Determination of: calcium salts, ferrous salts, hydrogen peroxide and expression of hydrogen peroxide solution concentrations in terms of the volumes of oxygen released; ferrous sulfate, menadione, paracetamol, nifedipine; sodium sulfite heptahydrate, ascorbic acid, ascorbyl palmitate, captopril; potassium permanganate, chloramine, ferric chloride; isoniazid and phenol.

Learning Objectives and Outcomes

The aim of this module is to familiarize students with the various types of volumetric analyses used in the pharmaceutical and health-related fields, as well as the technical operations required for their execution.

By the end of this module, students will be able to approach an analytical problem from both theoretical and practical perspectives and will therefore know how to correctly perform quantitative analysis using the most appropriate techniques, procedures, and precautions. Students will also be able to carry out basic laboratory operations, both manual and instrumental. Furthermore, they will be able to interpret specific monographs from the FUI XII and Ph. Eur. XII.

Module 2 (1.5 CFU)

Instrumental Analytical Methods

Electrochemical Methods of Analysis

Potentiometric determination of pH. Biamperometric determination of primary amino nitrogen: applications to the sulfonamides described in the FUI XII and Ph. Eur. XII and their supplements.

Optical Methods of Analysis

UV/Vis Spectrophotometry

General principles. Instrumentation. Quantitative analysis: selection of the working wavelength (λ), methods for concentration determination, and construction of calibration curves. Applications, with particular reference to monographs reported in the Ph. Eur. XII. Determination of chloramphenicol palmitate.

Spectrofluorimetry

General principles. Instrumentation. Quantitative analysis: methods for determining concentration.

Learning Objectives and Outcomes

The aim of this module is to provide students with the basic knowledge of selected instrumental analytical methods based on physicochemical principles. By the end of this module, students will be able to perform quantitative analysis of substances of pharmaceutical and health-related interest using electrochemical and spectroscopic techniques.

Laboratory Practical Sessions (1.5 CFU)

Quantitative analysis of substances included in the FUI XII and Ph. Eur. XII using volumetric and instrumental analytical methods.

1. E. Abignente, D. Melisi, M. G. Rimoli – Principi di analisi quantitativa DEI medicinali - Ed. Loghìa, Napoli.
2. G. C. Porretta - Analisi DI PREPARAZIONI FARMACEUTICHE. Analisi quantitativa. - Ed. CISU, Roma.
3. D. C. Harris - Chimica Analitica Quantitativa - Zanichelli, Bologna.
4. R. Cozzi, P. Protti, T. Ruaro - Analisi chimica: moderni metodi strumentali - Zanichelli, Bologna.
5. Vogel's Texbook of Quantitative Chemical Analysis - Fifth edition - Ed. Longman Scientific & Tecnical.
6. Farmacopea Ufficiale Italiana XII edizione.
7. European Pharmacopoeia XII edizione and supplements.
8. V.  Cavrini, V. Andrisano - Principi di analisi farmaceutica. Ed. Esculapio. Bologna
9. A. Carrieri - Manuale di Analisi Quantitativa dei Medicinali. EdiSES. Napoli

Learning will be assessed through a written examination (duration: 60 minutes), aimed at verifying the student's theoretical knowledge of the topics covered during lectures and their ability to represent in writing the chemical reactions involved in quantitative analysis through specific examples.

Exam dates are published on the Degree Program website: https://www.dsf.unict.it/it/corsi/lm-13/calendario-esami

The examination is intended to assess:

1. The fundamental theoretical knowledge of quantitative analysis (Descriptor 1).
2. The ability to apply theoretical principles to quantitative analysis, including methodological proficiency in applying various analytical techniques (Descriptor 2).
3. The aptitude for planning and carrying out a quantitative analysis strategy appropriate for the active ingredient being assayed, demonstrating the ability to choose the most suitable analytical procedures, validate the method, and analyze experimental results (Descriptor 3).
4. The ability to synthesize concepts and principles of quantitative analysis through chemical symbolism, using formulas and reaction equations, as well as the correctness and appropriateness of the scientific language employed (Descriptor 4).
5. The ability to independently integrate the information learned during the course (Descriptor 5).

The final grade will be determined by the arithmetic mean of the grades obtained in the two integrated courses: Analysis of Drugs and Health Products I and II.

Assessment may also be conducted remotely if circumstances require it.

ASSESSMENT CRITERIA

The final examination will be evaluated according to the following aspects:

Knowledge and Understanding

• Accuracy of theoretical knowledge.
• Completeness of the information provided.
• Ability to identify the analytical techniques involved.

Applied Skills

• Correct application of quantitative analysis procedures.
• Ability to interpret experimental data.
• Problem-solving skills in analytical contexts.

Independence of Judgment

• Ability to critically interpret results.
• Identification of possible experimental errors.
• Evaluation of the validity of the procedures adopted.

Communication Skills

• Correct use of scientific terminology.
• Clarity and coherence of explanations.
• Ability to establish connections between topics.

Learning Skills

• Ability to integrate knowledge from different parts of the syllabus.
• Appropriate use of bibliographic references and the prescriptions of the Italian Pharmacopoeia (F.U.I.).

GRADING SCALE

Grades are expressed on a 30-point scale according to the following criteria:

Failed Examination

The student does not possess the minimum required knowledge of the fundamental course contents, uses disciplinary terminology inappropriately, and is unable to apply the acquired knowledge.

Grade 18–21

The student possesses an essential knowledge of the main topics, demonstrates limited analytical ability, and uses simple but generally correct scientific language.

Grade 22–25

The student demonstrates a fair knowledge of the topics, is able to make simple connections between concepts, and can apply the fundamental analytical procedures.

Grade 26–28

The student demonstrates good preparation, correctly applies acquired knowledge, appropriately discusses analytical techniques, and uses adequate technical language.

Grade 29–30 with Honors

The student possesses a thorough knowledge of the topics, demonstrates strong critical thinking, independence of judgment, mastery of technical language, and the ability to solve complex analytical problems.

• Description of the quantitative determination of acetylsalicylic acid according to the European Pharmacopoeia, 12th edition.
• Description of the quantitative determination of nicotinamide according to the European Pharmacopoeia, 12th edition.
• Description of the quantitative determination of paracetamol according to the European Pharmacopoeia, 12th edition.
• Description of the quantitative determination of ferric salts according to the European Pharmacopoeia, 12th edition.
• Description of the quantitative determination of magnesium salts according to the European Pharmacopoeia, 12th edition.
• Description of the quantitative determination of calcium salts according to the European Pharmacopoeia, 12th edition.
• Description of the quantitative determination of citric acid according to the European Pharmacopoeia, 12th edition.
• Description of the spectrophotometric quantitative determination of chloramphenicol palmitate according to the European Pharmacopoeia, 12th edition.