Modern physico-chemical methods of analysis of organic compounds

The annual course of Professor Albert T. Lebedev, Ph.D., D.Sc.

The course is designated for post graduate students, probationers and postdocs of the Moscow State University. The course is 84 hours long. It starts from 1 November till 15 June. Besides the lectures on the most widely used physico-chemical methods of analysis of organic compounds, home tasks of structural elucidation based on the spectral information (10-15 unknowns), and seminars to discuss certain problems arising in NMR, IR and mass spectra elucidation constitute the course. In April-May all the students give their own lecture (45 minutes) dealing with a certain instrumental method. The course is terminated with an exam.

The program consists of two main blocks devoted to mass spectrometry and nuclear magnetic resonance spectroscopy.

Mass spectrometry

• Methods of ionization, separation and registration of ions.
• The main rules of fragmentation of organic compounds.
• The approaches to the interpretation of mass spectra. High resolution mass spectrometry. The main pathways of fragmentation of the principal classes of organic compounds in conditions of electron ionization.
• The use of databeases and spectral libraries for structural elucidation.
• Mass spectrometry in ecology (qualitative and quantitative analysis of ecotoxicants, mass chromatography, selected ion monitoring).
• Tandem mass spectrometry (main types of registration of spectra of metastable ions and collision activation spectra).
• Mass spectrometry of high molecular mass compounds and biomolecules (electrospray ionization, matrix assisted laser desorption/ionization).
• Fourie-transform mass spectrometry.
• Mass spectrometry in proteomics (analysis of proteins, elucidation of amino acids sequence in peptides, study of posttranslational modifications).

Nuclear magnetic resonance

• The basics (Fourie-transform NMR, Nyquist criterium, FID processing, phasing, foldings).
• Spin echo, refocusing of chemical shifts, J-spectroscopy (АРТ and its drawbacks).
• Polarization transfer (INEPT, DEPT - advantages and shortcomings).
• The principles of two-dimensional spectroscopy.
• 2DJ-spectroscopy (HOM2DJ, HET2DJ ¹H - ¹³C).
• Correlation 2D spectroscopy (COSY, COSY45, HETCOR, inversion 2D spectroscopy).
• Nuclear Overhouser effect (nature, practical consequences, homo- and hetero nuclear effect, technique of measurement, difference spectra, sample requirements).

Special lectures are devoted to the following methods:

• IR and UV- spectroscopy,
• photoelectron spectroscopy,
• electrochemical methods in organic chemistry,
• electron spin resonance,
• ion cyclotron resonance.