QUALITATIVE DRUG ANALYSIS
Academic year and teacher
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- Versione italiana
- Academic year
- 2022/2023
- Teacher
- REMO GUERRINI
- Credits
- 9
- Didactic period
- Secondo Semestre
- SSD
- CHIM/08
Training objectives
- Learning aims and objectives:
The aim of the course is to provide students with theoretical and practical knowledge useful for the recognition of molecules of pharmaceutical interest. The course will provide participants with the skills and abilities necessary to isolate and identify an active ingredient in pure form.
At the end of the course the student will be able to apply the analytical methods necessary to identify, from a qualitative-quantitative point of view, an active pharmaceutical ingredient included in the F.U. Italian monography. The student will be able to analyze the degree of purity of a drug, apply methods for the purification of drugs. The student will be able to perform analyzes useful for the identification of the functional groups of organic molecules. At the end of the course the student will be able to analyze and determine the structure of polyfunctional molecules. Prerequisites
- Entry requirements: inorganic chemistry, good knowledge of organic chemistry, analytical chemistry, techniques for the spectrometric identification of organic compounds, pharmaceutical chemistry. The practical knowledges acquired in the courses of General and Inorganic Chemistry, Organic Chemistry and Quantitative Drug Analysis are strictly required for a fruitful laboratory practice of this course.
Course programme
- Contents:
Chromatography: adsorption chromatography, partition chromatography, thin layer chromatography, column chromatography, high performance liquid chromatography.(HPLC) with the description of parameters and basic equations important for the theoretical plate number calculation.
Isolation and purification of sample: crystallization techniques, sublimation, distillation, liquid-liquid extraction.
Determination of physical properties: melting point, relative and absolute density, optical rotation, molecular weight, solubility.
Qualitative analysis for the elements: nitrogen, sulfur and halogens.
Elemental analysis: quantitative determination of C, H, N.
Identification of functional groups following colour test methods: ninhydrin, diazotization-copulation, ferric chloride, copper sulphate, Angeli and Rimini test, Tollens' reagent, Fehling' reagent. Preparation of crystalline derivatives of: acids, alcohols, aldehydes, ketones and amines.
Spectrometric identification of functional groups using: ultraviolet spectrophotometry, infra-red spectrophotometry, nuclear magnetic resonance spectroscopy.
Analysis and identification of some drugs included in the European Pharmacopea: antipyretic analgesics, xanthine derivatives, antibiotics, steroids, nicotinic acid derivatives, anaesthetics, antihistamine derivatives, barbiturate. Didactic methods
- Didactic organization: 32 hours of lessons in classroom concerning all the subjects reported in “Contents”. 8 hours will be employed to describe techniques for the isolation and the control of the purity grade of a substance. 6 hours will be employed to describe techniques for the determination of physical properties and elemental composition of substances. 12 hours will be employed to describe chemical and analytical procedures for the identification of functional groups. Finally, 6 hours will be employed to describe analytical methods reported in the European Pharmacopea useful for the identification of some drug classes.
60 hours of laboratory practice. This part of the course consists of at least 15 laboratory experiences performed in different days with a time of 4 hours. A workstation for each student will be available in the laboratory and the student will be assisted by a technician during the use of analytical instrumentations. Learning assessment procedures
- Type of exam: the exam is divided in two parts and each part carried out in different days. The first part, performed at the end of the laboratory practice, consists of the analysis of an unknown drug given to the student as pure compound. The object of this practical examination is to evaluate the practical ability developed by the student and to verify the level of knowledge and ability in the use of laboratory instrumentations. A time of 3 hours is lived to do this part of the exam. The use of books and internet is allowed. At the end of the analysis a written document describing in details the adopted analytical procedures and the final structure of the identified drug is required. A score of 3/6 is necessary to get over the practice part and pass to the second part of the exam. The second written part of the exam consist of a multiple choice tests in which 30 right answers, about themes treated in the course program, must be identified by the student in a set of 120 questions. In addition two open demands regarding theoretical aspects of the course will be administered to the student. A time of 90 minutes is lived to do this part of the exam. It is allowed to use only the calculating machine. A score of 15/30 is necessary to get over the theoretical part. The final score will be the result of the addition of the score obtained in the two parts of the exam. A final score of 36 will be evaluated as 30 with Lode. A positive score in the practical part of the exam will remain valid for 2 years.
Reference texts
- Bibliography references:
Farmacopea Ufficiale Italiana ed. XII
Manuale di Analisi Qualitativa. Giuseppe Caliendo; EdiSES.
Cavrini: Guida al riconoscimento di composti di interesse farmaceutico; Soc. Ed. Esculapio
Vogel: Chimica organica pratica; Casa Editrice Ambrosiana Milano
F.Savelli, O.Bruno: Analisi Chimico Farmaceutica Casa Editrice Piccin
Clarke's: Isolation and identification of drugs; The Pharmaceutical Press London
