Course syllabus
Drugs Analysis II
Overview
The course "Drugs Analysis II" and "Laboratory of Drugs Analysis II", conducted through the mediu of both face to face lessons and practical lab experiments, gives the student a basic grounding in the field of quality control quality control of drugs in bulk and in drug formulations. Specifically, the course aims to provide the student with the fundamental skills for the analytical aspects of process development, structural identification and characterization of drugs, for the control of their stability and the characterization and quantitative analysis of impurities. Analytical methodologies used in therapeutic drug monitoring, identification of counterfeit drugs and medicines, and analysis of biotechnological drugs will also be covered. To begin with, the analytical methods reported in the current Official Pharmacopoeia (with particular reference to the European Pharmacopoeia, EP) will be evaluated and then knowledge will be provided which will allow students to develop analytical procedures for the process development, control of the structural identity, purity control and stability of new chemical entities. The course then goes on an overview of the assays provided by EP for the quality control of plant drugs and related phytoderivatives (extracts and essential oils) and for the chemical and instrumental recognition of the active ingredients contained in them. The course also includes an overview of chemical-analytical methods for the quality control of drugs of biotechnological origin. Finally, methods applied to therapeutic drug monitoring and the identification of counterfeit drugs and medicines will be covered.
The practical laboratory experiments (which include mandatory exercises) provide students with the ability to identify unknown substances listed in EP through the application of chemical and instrumental methods
Program
- Introduction to the principles of pharmaceutical analysis according to EP
- Distinction between organic, metallo-organic and inorganic substances
- Solubility
- Elemental analysis.
- Chemical reactivity and functional group analysis: alkenes and alkynes, aromatic compounds, conjugated systems, alcohols, ethers, phenols, carbonyl compounds, carboxylic acids, esters, amides, amines, nitro compounds, sulfonic acids and sulfonamides.
- Specific recognition reactions for: amino acids and proteins, alkaloids, local anesthetics, antibiotics, barbiturates, carbohydrates and glycosidic derivatives, steroids, sulfa drugs, vitamins.
- Recognition reactions applied to individual drugs
- Derivatization reactions
- Stability studies
- Identification and characterization of impurities
- Identification of active principles in complex matrices
- Quality control of plant drugs and their derivatives (phytoextracts)
- Quality control of biotechnological drugs
2) Instrumental analysis: theoretical principles and applications to the recognition of substances listed in EP
- Solvent extraction, partition coefficient
- Sample preparation: application of extractive and chromatographic methodologies
- Determination of physical constants: melting point, density, refractometry and refractive index, polarimetry and determination of specific rotational power.
- Application of chromatographic, spectroscopic and spectrometric techniques for the identification and characterization of molecules of pharmaceutical interest and their impurities.
- Spectroscopic methods: UV/Visible, fluorescence, infrared spectroscopy.
- Criteria for selection and application of instrumental techniques in relation to the analytical problem.
Laboratory of Drugs Analysis II
Individual laboratory training
Recognition of organic and metallorganic substances of pharmaceutical interest
Introduction to the analysis of organic compounds. Organoleptic examination. Combustion tests and residue analysis, recognition of metals in organometallic substances registered in the F.U.
Preparation of Lassaigne's solution for the detection of nitrogen, sulfur, halogens, phosphorus. Solubility of organic substances: solubility in water and reactive solvents; classification of substances based on their solubility.
Assays for the recognition of functional groups in organic substances: alcohols, aldehydes, ketones, polyalcohols, sugars, carboxylic acids, α-oxyacids, phenols, amines, amino acids, esters, amides.
Examination of the substances registered in the F.U. Pharmaceutical substance classes: general and specific tests for alkaloids, sulpha, xanthine, glycosides, various substances.
Recognition of inorganic substances of pharmaceutical interest.
Prerequisites for admission
To conveniently attend the lessons, the student should possess basic knowledge of organic chemisty, medicinal chemistry and analytical chemistry.
Teaching Resources
- Slides available in myAriel - V. Cavrini - Guida al riconoscimento di composti di interesse farmaceutico - Esculapio Bologna - Vogel - Chimica Organica Pratica - Casa Editrice Ambrosiana - D. G. Watson - Analisi Farmaceutica - EdiSES s.r.l. Napoli - H. H. Bauer, G. D. Christian, J. E. O'Relly - Analisi strumentale - Piccin, Padova - R. Cozzi, P. Protti e T. Ruaro - Analisi chimica moderni metodi strumentali Vol I, II e III - Zanichelli Bologna. - R. Ugo - Analisi chimica strumentale - Editrice Scientifica Guadagni, Milano. - Kenneth A. Connors - A textbook of pharmaceutical analysis - John Wiley & Sons - F. Savelli, O.Bruno - Analisi Chimico Farmaceutica - Piccin
Assessment methods and Criteria
For each of the two teaching units, the learning assessment is evaluated by a mark out of thirty with a minimum grade of 18/30.
The final result will come from the average of the marks obtained in the two teaching units weighted by the credit value of each unit.
Teaching unit: Drug Analysis 2
The exam consists of a written test which is related to the topics covered in class, and is articulated in several points with exercises and open-ended questions with a final grade out of thirty. The written test lasts 120 minutes.
In order to be able to take the examination, it is essential to register for the exam session through the online SIFA service of the University. The outcome of the written exam will be published on the Ariel portal of Unimi.
Teaching unit: Laboratory of Drug Analysis 2
The Laboratory unit does not include an examination, but an acknowledgement of attendance, which is granted only if the student has correctly performed at least 50% of the unknown analyses. The overall evaluation of the activity performed by the student in the exercises included in the Laboratory unit is made on the basis of the results of the analyses and is expressed in thirtieths.
During a solar year, there will be seven exams and the students can take consecutive exams without any constraining.
