Drug Analysis

Course Description_Drug Analysis

SUBJECT:  DRUG ANALYSIS

 SYLLABUS of LECTURES

Winter semester 2024/2025

Term:                  Wednesday, 9:20 – 11:00, 15:45 – 17:25

Place:                  Room O419, 4^th floor, Odbojárov 10

Lecturer:            PharmDr. Iva Kapustíková, PhD.

1^st week: Drug analysis, content, and importance of the subject. The European Pharmacopoeia: General chapters, Monographs. European Directorate for the Quality of Medicines & HealthCare.

2^nd week: Qualitative analysis: Identification reactions of ions and functional groups.

3^rd week: Qualitative analysis: Identification reactions of organic drugs. Group reactions and selective reactions – Part I.

4^th week: Qualitative analysis: Identification reactions of organic drugs. Group reactions and selective reactions – Part II.

5^th week: Physical and physicochemical methods – General chapters in the European Pharmacopoeia – Part I.

6^th week: Physical and physicochemical methods – General chapters in the European Pharmacopoeia – Part II. Determination of acid-base properties and lipophilicity of drugs using instrumental methods.

7^th week: Purity of drugs and its control. Physical and physicochemical methods used in purity tests.

8^th week: Purity of drugs and its control. Limit tests for inorganic impurities.

9^th week: Quantitative analysis: Gravimetry. Volumetric methods in the European Pharmacopoeia – Part I.

10^th week: Quantitative analysis: Volumetric methods in the European Pharmacopoeia – Part II.

11^th week: Chemical analysis of drug substances. Quality control of the final pharmaceutical product. 

12^th week: Good manufacturing practice. Validation in pharmaceutical analysis. Technical norms. Pharmaceutical analysis in registration of medicinal products.

13^th week: Stability of medicinal products. Quality control of containers and materials used for the manufacture of containers. Computational exercises.

Bratislava 7^th September 2024

PharmDr. Iva Kapustíková, PhD.                                          doc. Mgr. Fils Andriamainty, PhD.                                                 

         responsible teacher                                                               head of department   

SUBJECT:  DRUG ANALYSIS 

SYLLABUS of LABORATORY PRACTICALS

Winter semester 2024/2025

Term:            Friday, 7:30 – 12:30    (27. 9., 11. 10., 25. 10., 8. 11., 22. 11., 6. 12.)

Place:            Laboratory O304 and O310a, 3^rd floor, Odbojárov 10

Teachers:     PharmDr. Iva Kapustíková, PhD.

1^st week: Qualitative analysis: Identification reactions of ions and functional groups – Inorganic ions.

3^rd week: Qualitative analysis: Identification reactions of ions and functional groups – Organic groups.

5^th week: Qualitative analysis: Identification reactions of drugs. Physical and physicochemical methods: Relationship between reaction of solution, approximate pH and colour of certain indicators; Potentiometric determination of pH; Conductivity. Preliminary test.

7^th week: Physical and physicochemical methods: Melting point – capillary method; Relative density; Refractive index; Optical rotation; Absorption spectrophotometry, ultraviolet and visible; Infrared spectroscopy; Thin layer chromatography.

9^th week: Purity of drugs and its control. Limit tests for inorganic impurities. Preliminary test.

11^th week: Quantitative analysis. Titrimetric methods.

INSTRUCTIONS for LABORATORY PRACTICALS

1.       During laboratory practicals, students must wear lab coats as well as bring their study literature and working aids, as appropriate. Students are obliged to follow all applicable safety rules when working in laboratory. They must keep their working place clean and tidy. Students inspect their workbenches, especially the content of the lockers, before the beginning of the laboratory practical and hand in their workbenches to the laboratory technician at the end of the laboratory practicals. Laboratory equipment and material, which is not included in workbench equipment is available in the preparation room upon registration of the student’s name and workbench number. All the borrowed equipment must be returned back to preparation room at the end of the practical. Students must always clean the fume hoods, scales, and all instruments after using them. They are asked to handle the glassware, scales, and instruments with care. In case it cannot be identified who is responsible for breaking a piece of glass usually used by all students, e.g. burette, cuvette, electrode, the whole group will have to cover the damage.

2.        Students have to note in detail their experimental results in order to be able to present them to the teacher on his request. Results obtained during the laboratory practicals are to be reported to the teacher who verifies them. After the results verification, students have to write a laboratory report. Theoretical knowledge and a readiness of the student for the laboratory work will be also verified by personal interview with the teacher during the practicals.

3.        Students are obliged to attend the complete laboratory practicals course. Any absence can be excused only in officially documented cases (medical certificate, etc.) or in case of serious family reasons. Absence can be excused only by the leading teacher of the laboratory practicals. The head of the department decides on sanctions in case of unexcused laboratory practicals absence. Two unexcused absences are considered to be a disciplinary offence followed by a proposal of the department to exclude the student from the course. Excused absences must be substituted on the dates and form assigned by the department.

4.      Two preliminary tests are taking place during the semester: in 3^rd and 5^th laboratory practicals. Scope of the 1^st test: European Pharmacopoeia, identification reactions of ions and functional groups, physical and physicochemical methods. Scope of the 2^nd test: identification of drugs, physical and physicochemical methods, purity of drugs, quantitative analysis. Maximal number of points is 10 = 100 % correct answers, student must obtain at least 60 % = 6 points in each test in order to pass it. In case the student does not pass one of the tests, he/she will take the first reparation preliminary test in the last week of the semester. In case student does not pass two of the tests, he/she will take a first reparation summary preliminary test in the last week of the semester. In the case the student does not pass first reparatory preliminary test in the last week of the semester, he/she has the opportunity to write a second reparatory preliminary test in January 2025. If student fails on second reparatory term, he/she must enrol the subject in the next academic year.

Bratislava 7^th September 2024

PharmDr. Iva Kapustíková, PhD.                                          doc. Mgr. Fils Andriamainty, PhD.                                                 

         responsible teacher                                                               head of department                                                                  

SUBJECT:  DRUG ANALYSIS

ORGANISATION of the FINAL EXAMINATION

Winter semester 2024/2025

Students must use university e-mail (the one ending with @uniba.sk) to communicate. There is no other way to validate their identity in the study process.

Conditions for admitting student to the final examination are as follows:

1.  successful graduation of 2 preliminary tests during the semester, i.e. at least 60 % in each test,

2.  100 % attendance at laboratory practicals.

Final examination is performed in written form. The exam consists of questions where all the content of Drug Analysis lectures and laboratory practicals will be represented. Student must obtain at least 60 % in order to pass exam. Scale of assessment (preliminary/final): 20/80.

The number of students registered for the final examination is unlimited. The registration for the final exam must be done via an AiS2 system only. The dates and organisation of the exam will be notified via AiS2 system according to current regulations.

Exams are divided to regular term, first and second reparation. If obtained score in the second reparation is lower than 60 %, student can enrol subject Drug Analysis next academic year.

Classification system: A: 100–92 %; B:  91–84 %; C:  83–76 %; D:  75–68 %; E:  67–60 %; FX:  <60 %.

Study materials:

• Lectures are available on Moodle.
• The European Pharmacopoeia. 11th Ed. Strasbourg: Council of Europe, 2022.
• Hansen, S., Pedersen-Bjergaard, S., Rasmussen, K.: Introduction to Pharmaceutical Chemical Analysis. Chichester: John Wiley & Sons, 2012.
• Kapustíková, I.: Drug Analysis, Laboratory Practicals. Bratislava: Comenius University in Bratislava, 2020.
• Kar, A.: Pharmaceutical Drug Analysis. New Delhi: New Age International, 2005.
• Pedersen, O.: Pharmaceutical Chemical Analysis. Methods for Identification and Limit Tests. New York: CRC Press, Taylor & Francis Group, 2006.
• Rouessac, F., Rouessac, A.: Chemical Analysis. Modern Instrumentation Methods and Techniques. 2nd Ed. Chichester: John Wiley & Sons, 2007.
• Watson, D. G.: Pharmaceutical Analysis. A Textbook for Pharmacy Students and Pharmaceutical Chemists. 4th Ed. Edinburgh: Elsevier, 2017. 

Bratislava 7^th September 2024

PharmDr. Iva Kapustíková, PhD.                                          doc. Mgr. Fils Andriamainty, PhD.                                                 

         responsible teacher                                                               head of department                                                                    

Kapustíková, I.: Drug Analysis, Laboratory Practicals. Bratislava: Comenius University in Bratislava, 2020. ISBN 978-80-223-5055-6.