Modern Structural Methods   (256H2)

Academic year:

2023/2024.

Attendance requirements:

There are no requirements.

ECTS:

9

Study level:

Study programs:

Teacher:

Ljubodrag V. Vujisić, Ph.D.
associate professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Assistants:

Gordana B. Krstić, Ph.D.
assistant professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Ivana V. Sofrenić, Ph.D.
assistant with PhD, Faculty of Chemistry, Studentski trg 12-16, Beograd

Hours of instruction:

Weekly: four hours of lectures + two hours of exercises + three hours of labwork (4+2+3)

Goals:

Students should get acquainted with the following areas of instrumental methods:

1. Multipulse 1D, 2D and 3D NMR methods (H,H-COSY, TOCSY, H,H-NOESY, ROESY, HETCOR, INADEQATE, and selected 3D experiments), semi-solid state NMR (HR-MAS NMR) as well as their application.
2. Basic principles of tandem mass spectrometry (MS/MS) and its application in analytics.
3. Application of MS to determine the structure of thermolabile molecules such as, polypeptides, sugars, etc.

Outcome:

Students will be trained for solving the structures of complex organic molecules using multi-pulsed NMR experiments. They will acquire the necessary knowledge and skills to identify and quantify them using modern mass spectrometry methods.

Teaching methods:

Lectures, theoretical exercises, labwork, homework and colloquia.

Extracurricular activities:

Guest lectures.

Coursebooks:

1. Slobodan Milosavljević: Strukturne instrumentalne metode
2. Vele Tešević: Osnove masene spektrometrije organskih jedinjenja
3. Ernö Pretsch, Philippe Bühlmann and Martin Badertscher: Structure determination of organic compounds, Tables of Spectral Data
4. L. D. Field, S. Sternhell, J. R. Kalman: Organic structures from spectra, fourth edition

Additional material:

—

Lectures:

0 points (4 hours a week)

Syllabus:

1. Multipulse 1D and 2D NMR methods.
2. H,H-COSY, TOCSY.
3. Pulse sequences for suppression of signal in the spectrum (watergate, CPMG).
4. H,H-NOESY, ROESY.
5. HETCOR.
6. INADEQATE.
7. Protein-ligand screening STD (saturation transfer difference) NMR.
8. Selected 3D NMR experiments.
9. Insoluble Substance Analysis - Semi-solid NMR, HR-MAS assay.
10. Soft ionization methods in MS.
11. Tandem mass spectrometry (quadrupole, ion trap, ion cyclotron, orbitrap, etc.).
12. MS/MS experiments of qualitative and quantitative targeted analysis (MRM, SRM, daughter scan and neutral loss).
13. Electronic Paramagnetic Resonance (EPR) - Basic Principles and Application.

Exercises:

0 points (2 hours a week)

Labwork:

10 points (3 hours a week)

Syllabus:

1. Structure elucidation of organic compounds based on H,H-COSY and TOCSY spectra.
2. Structure elucidation of organic compounds based on HETCOR spectra.
3. Structure elucidation of organic compounds based on INADEQATE spectra.
4. Structure elucidation s of organic compounds based on H, H-NOESY and ROESY spectra.
5. Introduction to the existing equipment of the Faculty of Chemistry (GC, LC, MS, GC/MS, LC/MS); sample preparation, spectra capture and interpretation. NMR, 2D NMR).
6. Antioxidative activity (DPPH radical assay) of various sample types.
7. HPTLC - Bioautography assay.
8. Methods for fraud detection in food supplements.
9. Secondary structure determination of proteins using FTIR spectroscopy.
10. Quantitative NMR analysis (qNMR).
11. STD NMR spectroscopy: Protein-ligands screening.
12. NMR in quality control of Heparin Sodium.

Colloquia:

30 points

Written exam:

30 points

Oral exam:

30 points