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, etc.

The learning assessment consists in a written exam (2 hr) 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) and two calculation exercises (up to a maximum of 10 points in total).

•Pharmaceutical analysis: general aspects, phases constituting the qualitative-quantitative analysis; concept of matrix, sample, interfering substances. Types of samples in drug analysis. Criteria for choosing the analytical technique based on the sample to analyse. Purpose of qualitative-quantitative analysis and areas of use in the pharmaceutical field.
• Strategies for the identity confirmation of some drugs inscribed in the European Pharmacopoeia: wet chemistry, solubility, thin layer chromatography (TLC), polarimetry (general and instrumental aspects of the technique, optical rotation, specific optical rotation, optical purity), determination of the melting point (experimental aspects of the technique; melting range of pure and mixtures of substances).
• Analytical methods based on light absorption, UV-Vis spectrophotometry: general aspects, Beer's law: inherent limitations, instrumental and chemical deviations. Quantitative analysis: general aspects, calibration curves. Instrumental aspects: light sources and detectors. Calibration of a spectrophotometer according to the European Pharmacopoeia. Methods based on light emission, photoluminescence: fluorescence and phosphorescence. Spectrofluorimetry: general aspects. Excitation and emission spectra. Beer's law applied to fluorimetry, calibration curves. Quantitative fluorimetric analysis: operative principles.
• Reactions involved in the degradation of drugs: Definition of impurity and degradation products.
• Calculations in pharmaceutical analysis. Resolution of problems concerning the analysis of active ingredients and their formulations
• Chromatographic methods: HPLC: parts constituting of an HPLC system: pumping system; isocratic and gradient elution modes. Eluents. Spectrophotometric, fluorimetric, electrochemical, mass spectrum detectors: operating principles and applications. Stationary phases: silica and silica chemically modified silica to obtain different types of selectivity. Characterization of chromatographic peaks. Tailing and its objective measure. Theoretical plates number. Resolution. Role of pH in HPLC analysis: ion suppression and ion pair. Calculations related to the preparation of buffer solutions. Operational parameters of an HPLC analytical procedure.
• Development and validation of analytical methods according to international guidelines.
• Stability studies of drug substances (active ingredients) and drug products: studies purposes, long term and accelerates protocols, on-going stability studies.

LABORATORY ACTIVITIES:
Determination of average weight and weight uniformity. Determination of the active ingredient (Fe2+) in a formulation of ferrous gluconate in sachets. Determination of the impurity (Fe3+) in a formulation of ferrous gluconate in sachets. Determination of loss on drying using thermogravimetric balance. Determination of pH of a pharmaceutical powder when reconstituted in aqueous solution. Determination of percent content of troxerutin in drug substance.

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.