ANALISI FARMACEUTICA E NUTRACEUTICO-ALIMENTARE 1 A - L

The course aims to provide the student with basic knowledge relating to the nature, denomination, determination of the chemical composition and quantitative determination of analytes, understood as:

- inorganic and organic pharmaceutical compounds;

-food products relating to the non-nutritional, but functional and therapeutic component;

- nutraceutical products and food supplements.

The aim of the course is to provide the assumptions underlying the use of substances of pharmaceutical interest, food supplements and nutraceuticals in the management of health and prevention of deficiency states.

The course, which includes both classroom lessons and laboratory practice, is divided into two modules (Module A and Module B).

 

In accordance with the five Dublin Descriptors, upon completion of the course, the student:

1.   Knowledge and understanding

-        will be able to describe the structures of the main chemical compounds found in pharmaceutical formulations, functional foods, dietary supplements, and nutraceuticals;

-        will be able to describe the instrumentation and glassware required to perform the considered analytical methods.

Assessment methods: questions in the written exam and evaluation of practical laboratory activities.

2.   Applying knowledge and understanding

-        will be able to perform manual and instrumental chemical analyses for qualitative identification purposes, and apply analytical methods to both pure analytes and mixtures.

-        will be able to demonstrate knowledge and understanding of the main volumetric and spectrophotometric analytical methods, as well as the ability to perform them in the laboratory;

Assessment methods: questions in the written exam and evaluation of practical laboratory activities.

3.   Making judgements

-        will critically evaluate and interpret the results of identification reactions performed in the laboratory on unknown mixtures, discussing the procedural aspects;

-        will be able to provide a critical evaluation of the analytical methods available for the quantitative determination of substances of pharmaceutical or nutraceutical/food interest, with reference to the monographs in the Italian and European Pharmacopoeias.

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

4.   Communication skills

-        will appropriately present and discuss experimental data by drafting a clear, descriptive report of the practical experiments conducted in the laboratory.

Assessment methods: terminological accuracy and descriptive clarity in both the written exam and laboratory reports.

5.   Learning skills

-        will develop the skills necessary to independently deepen his/her expertise regarding the qualitative and quantitative characterization and use of substances of pharmaceutical and nutraceutical interest for the prevention of deficiency states.

The course includes Theoretical Lectures (LT) in the classroom and individual practical exercises in the laboratory.

 

According to the RDA, Art. 12 - University Training Credits (CFU), the standard 25-hour workload of the student, corresponding to one credit, may include:

a) 7 hours dedicated to lectures or equivalent teaching activities and the remainder to individual study;

b) at least 12 and no more than 15 hours dedicated to classroom exercises or equivalent supervised activities (lab practice) and the remainder to personal study and reworking.

 

Module A – First semester – Prof. Valeria Pittalà

 

Frontal lectures (3 CFU, delivery-based and interactive teaching): all course topics are presented, and students are actively called upon to participate in discussions.

Practical exercises (1.5 CFU, interactive teaching): the student performs qualitative determinations and is encouraged to engage and compare results with colleagues and the instructor.

Laboratory reports: At the end of each exercise, the student drafts a report, which is evaluated and commented on by the instructor during the subsequent session.

 

Module B – Second semester – Prof. Giuseppe Romeo

 

Module B activities are constituted by class lectures and case studies (3 CFU, delivery-based and interactive teaching) along with laboratory practice (1.5 CFU, interactive teaching).

During class lectures, all course content is presented in detail. Students are asked to actively discuss presented topic and 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.

 

Should teaching be carried out in mixed mode or remotely, it may be necessary to introduce changes with respect to previous statements, according to the course content outlined in the syllabus

For effective participation in the course, basic knowledge of the following subjects is essential: general chemistry (solution equilibria, acidity and basicity, pH, oxidation states, standard potentials, redox reactions), organic chemistry (characteristics and reactivity of the main classes of organic compounds), and analytical chemistry (theoretical aspects of volumetric and spectrophotometric analytical methods, as well as complexation and chelation).

Formal prerequisites: General and Inorganic Chemistry, Organic Chemistry 1.

Attendance is mandatory in accordance with the degree regulations of the Single-Cycle Degree Course in Pharmaceutical Chemistry and Technology. Absence is permitted for no more than 30% of the total lecture hours, evaluated across all delivery formats (https://www.dsf.unict.it/it/corsi/lm-13_ctf/regolamento-didattico).

Module A – First Semester - Prof. Valeria Pittalà

 

Introduction to the theoretical and practical course: general rules for good laboratory practices and safety; types of hazards; hazard and precautionary statements; knowledge of safety pictograms; personal protective equipment (PPE); special waste disposal.

Overview of the fundamental theoretical principles of qualitative analysis: chemical composition and physical form of analytes; solutions, solubility, precipitates, and solubility product; acid-base solutions and pH; introduction to complexation and the stability of complexes.

Overview of sample treatment methods: classification of the sample's nature, preliminary treatments, purification, separation of a mixture, and extraction methods.

Overview of analytical methods and semi-micro reactions: applications outlined by the Italian (F.U.I.) and European Pharmacopoeias, precipitation, solubilization, oxidation-reduction (redox), and complexation.

Overview of instrumental methods: theoretical principles of the optical and chromatographic methods used in the laboratory.

Practical laboratory exercises: including dry and wet identification methods for inorganic, anionic, and cationic analytes, both in pure form and in mixtures, as well as the use of chromatographic methods such as TLC (Thin-Layer Chromatography).

 

Module B – Second semester – Prof. Giuseppe Romeo

 

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. Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia 12th.

Complexometric titrations. Titration methods. Preparation and standardization of an EDTA solution. Metallochromic indicators. Examples of applications, with particular reference to calcium and magnesium compounds and the relevant monographs in the Italian Pharmacopoeia XII ed. and the European Pharmacopoeia 12th.

Oxidation-reduction titrations. Permanganometry, cerimetry, iodimetry, iodometry, bromometry.

Applications with reference to monographs in Italian Pharmacopoeia XII ed. and European Pharmacopoeia 12th.

Electroanalytical methods

Potentiometric determination pH. Potentiometric detection of the end-point in titrations. Biamperometric determination of primary aromatic nitrogen: applications described in Italian Pharmacopoeia XII ed. and European Pharmacopoeia 12th.

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 12th.

Fluorimetry. Principles and basic features of the technique, instrumentation, applications to the quantitative analysis of pharmaceutical substances.

 

The Module B 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:

1. Consignment of the work station. Safety in laboratory. Glassware and analytical balance usage.
2. Titre determination of a NaOH solution. Utilization of acid-base indicators.
3. Standardization of a HCl solution by means of anhydrous Na₂CO₃ as primary standard.
4. Quantitative determination of an unknown Na₂CO₃ sample through an acidimetric titration.
5. Standardization of a NaOH solution by means of a suitable primary standard.
6. Quantitative determination of an unknown L-(+) tartaric acid sample through an alkalimetric titration.
7. Quantitative determination of an unknown ascorbic acid (vitamin C) sample through an iodimetric titration.
8. Determination of total hardness in drinking water. Determination of mg/L of Ca⁺⁺ ion and Mg⁺⁺ ion.
9. Determination of per cent purity of a caffeine sample by UV spectrometry. Beer-Lambert law use.
10. pHmeter calibration and use. Potentiometric detection of the end-point in a neutralization titration. Construction of the titration curve.
11. Quantitative determination of an unknown caffeine sample by UV spectrometry. Construction of the calibration line.

Module A – First semester – Prof. Valeria Pittalà

1. Araneo A. Chimica analitica qualitativa. Metodo periodale. Ambrosiana Milano Ed. 1993, ISBN 9788808080189
2. L. Mannina, M. Daglia, A. Ritieni. La Chimica e gli alimenti: nutrienti ed aspetti nutraceutici, C.E.A. (2019), ISBN 9788808184948
3. Cavrini V., Andrisano V. Principi di Analisi Farmaceutica. Esculapio ed. 2018, ISBN: 9788893850322
4. Cappelli P., Vannucchi V. Chimica degli Alimenti, conservazione e trasformazione. Zanichelli ed. 2006, ISBN 9788808621238
5. Farmacopea Ufficiale Italiana and European Pharmacopoeia last editions.
6. Teaching materials and lecture slides provided by the instructor on the university's e-learning portal.

 

Module B – Second semester – Prof. Giuseppe Romeo

1. E. Abignente, D. Melisi, M. G. Rimoli – Principi di analisi quantitativa dei medicinali - Ed. Loghìa, Napoli, 2011. ISBN 978-88-95122-21-2
2. A. Carreri - Manuale di Analisi Quantitativa dei Medicinali – EdiSES, Napoli, 2019. ISBN 978-88-3319-004-0
3. D. C. Harris - Chimica Analitica Quantitativa - Zanichelli, Bologna, 2017. ISBN 978-88-08-82105-8
4. A. I. Vogel, Vogel's Texbook of Quantitative Chemical Analysis - Fifth edition - Ed. Longman Scientific & Technical, Harlow (England), 1989. ISBN 0-582-44693-7
5. Farmacopea Ufficiale Italiana XII edizione. Istituto Poligrafico e Zecca dello Stato, Roma, 2008. ISBN 978-88-240-2884-4
6. European Pharmacopoeia 12th edition. EDQM Publication, Strasbourg (France), 2025. ISBN 978-92-871-9611-8

 

Module B. Items 1 and 2 are textbooks, 3 and 4 are reference books, Italian and European Pharmacopoeias (item 5 and 6) are the sources for official quantitative analyses of pharmaceuticals.

 

The final exam is a written test, consisting of both open-ended and multiple-choice questions; its duration is designed to evaluate the assimilation of the contents from both modules aimed at ascertaining the student's level of knowledge, comprehension, and critical analysis skills.

To take the exam, students must register online via the Student Portal (exam schedule: http://www.dsf.unict.it/corsi/lm-13_ctf/calendario-esami). The registration list opens approximately fifteen days prior to the scheduled exam date.

 

The final grade is expressed out of thirty (trentesimi) according to the following grading scale:

Fail (Non idoneo): Significant deficiencies in knowledge and understanding of the topic; irrelevant analytical skills.

18-20: Modest knowledge, evident imperfections, barely sufficient analytical skills.

21-23: Just above sufficient knowledge, fair analytical and synthesis skills.

24-26: Good knowledge, good analytical skills, and logical argumentation.

27-29: More than good knowledge, notable synthesis skills, appropriate use of standard references.

30-30 cum laude (30-30 e lode): Excellent knowledge, outstanding synthesis skills, and significant critical insights.

 

Learning assessment may also be carried out on-line, should the conditions require it.

 

Information for students with disabilities and /or SLD

 

To ensure equal opportunities and in compliance with current laws, interested students may request a personal interview in order to plan any compensatory and/or dispensatory measures based on educational objectives and specific needs. Students may also contact Prof. Santina Chiechio (santina.chiechio@unict.it) in her capacity as the CInAP (Center for Active and Participatory Inclusion – Services for Disabilities and/or Specific Learning Disorders; https://www.cinap.unict.it/content/referenti) representative for the Department of Drug and Health Sciences.

 

 

Module A – Prof. Valeria Pittalà

Discuss the Italian Official Pharmacopoeia and the European Pharmacopoeia.

What are Material Safety Data Sheets (MSDS)?

Describe the identification methods for an ion via dry testing (via secca), a cation via wet testing (via umida), and an anion via wet testing.

Writing and balancing neutralization, complexation, and oxidation-reduction (redox) reactions.

Examples of extraction methods for plant-based nutraceutical products.

 

Module B – Prof. Giuseppe Romeo

Description of the general features of a volumetric analytical technique.

Description of the quantitative analysis of acetylsalicylic acid according to EP 12th.

Description of the quantitative analysis of paracetamol according to EP 12th.

Description of % nitrogen content determination in pharmaceutical and food compounds.

Description of the quantitative analysis of magnesium ions in the presence of calcium ones.

Description of the quantitative analysis of primary aromatic amino-nitrogen according to EP12th.

Description of the spectrophotometric quantitative analysis of prednisolone acetate according to EP 12th.

What do accuracy and precision refer to in a quantitative analysis?

What are the features of primary standards?

How do you standardize a ceric sulphate solution?