Ateneo - UPO

The course will deal with the main aspects of the pharmaceutical analysis.
• General aspects of pharmaceutical analysis, classification of the various types of samples and techniques applied to their preparation for analysis.
• Methods of analysis for the identification of drugs: solubility, melting point, optical rotation, infrared spectrometry (IR) and TLC.
• Drug chemical stability: forced degradation studies and stability studies of drug substances and drug products.
• Analytical methods for the quali-quantitative analysis of drugs: spectrophotometry UV-Vis and spectrofluorimetry; theoretical and instrumental aspects; method development.
• Chromatographic methods. HPLC: theoretical and instrumental aspects; method development.
• Calculation in pharmaceutical analysis.
• Laboratory practices: identification of drugs whose monograph are reported in the current European Pharmacopoeia; determination of the content of the active pharmaceutical ingredients in drug substance and drug products.

• European Pharmacopoeia (Ph. Eur.) current edition.
• Analisi Chimico Farmaceutica F. Savelli, O. Bruno – Piccin, Padova.
• Analisi Farmaceutica D.G. Watson – EDRA LSWR, Milano.
• Analisi Farmaceutica Qualitativa A. Carta, M.G. Mamolo, F. Novelli, S. Piras – Edises, Napoli.
• Manuale di Analisi Qualitativa G. Caliendo – Edises, Napoli.
• Principi di Analisi Farmaceutica. V. Cavrini, V. Andrisano – Società Editrice Esculapio, Bologna.
• Chimica Analitica Quantitativa. D.C. Harris –Zanichelli.

By attending the course, the student will acquire the basic skills on the main analytical techniques employed in the pharmaceutical analysis laboratories and utilized to evaluate the stability of drugs, so implementing the regulatory agencies guidelines. The laboratory activities allow the student to apply the analytical methods to real pharmaceutical samples. In addition, the proposed calculation exercises allow the student to calculate and properly evaluate the results obtained during lab activities.

For a successful attendance of the course, students must have satisfied the prerequisites provided for by the regulations of the degree course in CTF (Article 34):
1) to enroll in the third year the student must have passed all the first year exams
2) to attend the Drug Analysis II course (theoretical and practical part) it is mandatory to have attended the Drug Analysis course I (theoretical and practical part) and to attend the exam sections it is mandatory to have passed the Analytical chemistry and methods in drug analysys and Drug analysis I.
It is preferable to have the basic knowledge for using Microsoft Excel software for statistical analysis.

Frontal lessons and laboratory activities.
The theoretical lessons will be held mainly with the support of slides projected in the classroom. The exercises related to calculations in pharmaceutical analysis will be treated in the classroom by resolution of real problems taken from the pharmaceutical field.
The laboratory activities will be carried out in laboratories equipped with the analytical instrumentation suitable for the pharmaceutical analysis in the field of quality control: UV and FTIR spectrophotometers, polarimeter, melting point equipment, thermogravimetric balance, Karl Fischer titrator etc.

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.

The learning assessment consists in a written exam (2 hours) plus the evaluation of the results obtained in the laboratory activities.
The written part (minimum mark: 17 points) consists of: 10 questions (T/F, multiple choice questions, open question: 1.6 points each, with the partial evaluation of the response), two questions (2.5 points each), problems (up to a maximum of 10 points in total).

• General aspects of the quali-quantitative pharmaceutical analysis: concept of sample, analyte, matrix, interfering substances, types of samples and objectives in drug analysis. Criteria for the selection of the analytical technique based on the sample to analyse. • Strategies for the identity confirmation of some drugs registered in the European Pharmacopoeia: wet chemical analysis, solubility, thin layer chromatography (TLC), polarimetry (fundamentals and operative aspects of the technique, optical rotation, specific optical rotation, optical purity), determination of the melting point (fundamentals, melting range of pure and mixtures of substances). • Analytical methods based on light absorption, UV-Vis spectrophotometry: properties of the electromagnetic waves and the chromophores. Fundamentals: sources, wavelength selectors, cuvettes, and detectors. Beer's law and its deviations, isosbestic point, calibration of a spectrophotometer according to the European Pharmacopoeia. Operating procedures for qualitative-quantitative analysis (calibration curves), Methods based on light emission; photoluminescence: fluorescence and phosphorescence, Jablonsky diagram. Fluorescence spectroscopy: fundamentals, Beer's law applied to the fluorimetry, fluorescence measurements (emission, excitation, fixed wavelength, synchronous spectra). • Generalities on the assays and analytical controls of drug substances and drug products: average mass and uniformity of mass, uniformity of content, loss on drying, determination of moisture by Karl-Fischer method. Definition of impurities and degradation products, main reactions involved in the degradation of drugs. • HPLC chromatographic methods: fundamentals, constituent parts of an HPLC system, types and features of the stationary phases (silica and chemically modified silicas to obtain the different selectivity), mobile phase (eluent system), elution in isocratic and gradient modes, control of the pH of the mobile phase using buffers (ion suppression and ion pairing), principal detectors (UV-Vis, PDA, FLD, MS, RID, electrochemical, ELSD, CAD). Quantitative analysis: internal standard, external standard, standard additions. Parameters for the evaluation of the chromatographic system performance: capacity factor, selectivity, efficiency, theoretical plates, resolution, asymmetry and tailing factor, band broadening theory for liquid chromatography. • Generalities on sample preparation techniques for pharmaceutical analysis: liquid-liquid extraction (LLE), liquid-liquid extraction on solid support (SLLE), solid phase extraction (SPE), other techniques. • Stability studies of drug substances and drug products: purpose of long-term and accelerated stability studies and their implementation according to ICH guidelines, on-going stability studies, forced degradation studies. • Validation of analytical procedures according to the ICH guidelines. • Pharmaceutical analysis calculations: development of formulas for determining the content of the active ingredient in pharmaceutical formulations, determination of the drug substances purity, buffer solutions preparation.

LABORATORY ACTIVITIES PART A. Identity confirmation of some drugs registered in the European Pharmacopoeia.

LABORATORY ACTIVITIES PART B. Determination of average weight and weight uniformity. Quantitative determination UV-Vis of the active ingredient (Fe2+) and the related impurity (Fe3+) in a formulation of ferrous gluconate. Determination of the purity (Fe2+ assay) of a batch of ferrous gluconate. Determination of loss on drying using thermogravimetric balance. Determination of pH of a pharmaceutical powder when reconstituted in aqueous solution. Quantitative determination UV-Vis of troxerutin in drug substance. Determination of moisture by Karl-Fischer method.

At the end of the course, which also includes laboratory activities, the student will have the knowledge of the main analytical techniques used to determine the purity of active pharmaceutical ingredients and their potency in the corresponding formulations also in the context of stability studies. Furthermore, the student will be able to calculate, interpret and evaluate the analytical data obtained.