Ateneo - UPO

Techniques Used in the Quantitative Pharmaceutical Analysis of Drugs: *Principles of volumetric analysis (titrations) in aqueous and –briefly– in non-aqueous media.
*UV-Vis spectrophotometry and Fluorimetry *Calculations in pharmaceutical analysis
*Chemical stability of drugs

* E. Abignente, D. Melisi, M.G. Rimoli, “Principi diAnalisi quantitativa dei medicinali”, Loghìa.
* D. S. Hage, J. D. Carr, “Chimica analitica e analisi quantitativa”, Casa Editrice Piccin, edizione italiana
* Vogel, “ Analisi chimica quantitativa”, Casa Editrice Ambrosiana
* D.C. Harris, “Chimica Analitica Quantitativa”, Zanichelli.
* Skoog and West, “Chimica Analitica”, EdiSES
* F.Savelli-O. Bruno, “Analisi chimico farmaceutica”, Casa editrice Piccin Padova
* D.L. Pavia, G.M. Lampman, G.S. Kriz, “Il laboratorio di chimica organica”, Edizioni Sorbona Milano

The course will give the student the first notions concerning the main techniques used in chemical laboratories. After the theoric part will follow some practical exercises in order to deepen the topics and to allow the student to acquire the basic handedness useful in laboratory.

There are no specific prerequisites although the knowledge of the basic notions of the main chemical reactions and general chemistry are very important. It is however necessary to follow the entire course and then to take the exam to be in compliance with the prerequisites provided for in the study plan.

The course comprises traditional lectures (in-class instruction), active learning components (classroom exercises and practical laboratory sessions), and experimental interactive learning (self-paced activities available at all times on the DIR platform). All teaching activities will be delivered in person; if necessary and only in exceptional cases, synchronous remote lessons may be conducted.

Students with physical disabilities, Learning Disabilities or Special Education Needs can request specific services and tools via the Staff Sviluppo e Coordinamento Carriere e Servizi alle Studentesse e agli Studenti, consulting the University webpage: https://www.uniupo.it/en/services/services-students-physical-or-learning-disabilities

Students with disabilities, learning disabilities or special education needs, once they have contacted the University Staff, can refer to the tutor in charge of the course to define the examination modalities, concerning academic aspects.

* In-itinere Assessment Tests (Mandatory)
During the course, 3 mandatory in-itinere assessment tests are scheduled for self-assessment and learning progress monitoring:
1. Entry Test (Laboratory - Theory): Multiple-choice / true-false questions + 2 problems on concentration calculations (Duration: 30 min).
2. In-itinere Test (Laboratory - Practice): 2 problems related to the practical lab experiments (Duration: 30 min).
3. In-itinere Test (Classroom - Post-laboratory): 1 problem on Official Pharmacopoeia (FU) volumetric titrations and theory + 1 problem on instrumental analysis and theory (Duration: 1 hour).

* Laboratory Bonus Points (Max 2 points)
Based on the evaluation of activities and data submitted during the laboratory sessions, 0 to 2 bonus points will be awarded and added directly to the final written exam score.

*Final Written Exam and Overall Grade
The final exam consists of a written test whose structure mirrors that of the in-itinere assessment tests.
Written exam grade: Max 30 points.
Final grade: Written exam grade + Laboratory bonus points (max 2 points).
Honors (Cum Laude): Awarded with a total score equal to or higher than 30.5.

Quantitative Analysis:
Overview and types of pharmaceutical analysis
Phases of an analytical method
Methods of expressing concentration
Significant figures
Mass determination: analytical and technical balances
Concentration expression methods
Volumetric Analysis:
Volume determination: methodology and instrumentation (burette, volumetric flask, graduated pipettes, Erlenmeyer flasks, beakers, cylinders)
Concept of titration: direct and indirect titration
Standard solutions and primary standards
Determination of titration endpoint: equivalence point, end point, titration error
Concept of indicators
Chemical reactions involved in titrations
Acid–Base Titrations:
Titration curves: influence of titrant/ analyte concentration and pKa
Common titrants:
Acidimetry: HCl, H₂SO₄, HClO₄; primary standards: Na₂CO₃, HgO Alkalimetry: KOH, NaOH; primary standards: KHIO₃, potassium hydrogen phthalate, benzoic acid; Endpoint determination; Theory of indicators: transition range, single-color indicators (e.g., phenolphthalein) and dual-color indicators (e.g., methyl orange)
Redox Titrations: Titration curves: influence of titrant/ analyte concentration and redox potential; Endpoint determination using potentiometric methods and redox indicators (e.g., ferroin); Permanganometry: KMnO₄ standard solutions – preparation, stability, standardization, analytical reactions

Instrumental Analysis:
UV-Vis Spectrophotometry: Beer’s Law and its deviations; Spectrophotometer calibration according to the European Pharmacopoeia; Quantitative analysis via calibration curves Fluorimetry: Instrumental aspects; Beer’s Law as applied to fluorimetry High-Performance Liquid Chromatography (HPLC): Overview and components of an HPLC system; Types and properties of stationary phases: Mobile phase (eluent system): isocratic and gradient elution; pH control using buffer solutions; Common detectors; Use of internal standard, external standard, and standard additions; System performance parameters Gas Chromatography (GC): Overview and components of a gas chromatograph; Selectivity, efficiency, resolution, retention indices; Headspace techniques: static, dynamic, and SPME. Mass Spectrometry (MS) for Quantitative Analysis: Ion sources, resolving power, resolution; Acquisition modes: full scan, SIM, MS/MS; Use of spectral libraries. Coupled Techniques: GC-MS (Gas Chromatography–Mass Spectrometry) and HPLC-MS (Liquid Chromatography–Mass Spectrometry): Interface and coupling challenges
Pharmaceutical Analysis Exercises:
Problem-solving related to: Titration calculations; Formula development for determining active ingredient content in pharmaceutical formulations; Purity determination of active pharmaceutical ingredients
Laboratory Sessions (1 CFU – 16 hours):
Preparation and standardization of a NaOH solution
Determination of citric acid purity
Quantitative determination of acetic acid
Quantitative determination of hydrogen peroxide
UV-Vis quantitative determination of the active ingredient (Fe²⁺) and impurity (Fe³⁺) in a ferrous gluconate formulation
Purity determination (Fe²⁺ content) of a batch of ferrous gluconate API
UV-Vis quantitative determination of a pharmaceutical active ingredient

By the end of the course, the student is expected to:
Acquire practical skills to perform basic quantitative analyses, including instrumental techniques; Be able to solve problems related to volumetric and instrumental quantitative analysis; Critically interpret and discuss quantitative data reported in the scientific literature