IC151 Solid State NMR in Pharmacology

Faculty of Science
Spring 2016
Extent and Intensity
1/0/0. 1 credit(s) (plus extra credits for completion). Type of Completion: z (credit).
Teacher(s)
doc. Elina Sievanen (lecturer), prof. RNDr. Radek Marek, Ph.D. (deputy)
Guaranteed by
prof. RNDr. Radek Marek, Ph.D.
Department of Chemistry – Chemistry Section – Faculty of Science
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science
Course Enrolment Limitations
The course is offered to students of any study field.
Syllabus (in Czech)
  • Nuclear magnetic resonance spectroscopy is a technique, wherein a sample is placed in a homogeneous magnetic field, irradiated, and a magnetic signal detected. In addition to other factors, the relative orientation of the molecule with respect to the axis of the field affects the signal. In a classical liquid-state NMR experiment, Brownian motion leads to an averaging of anisotropic interactions. In media with no or little mobility, however, chemical shift anisotropy (CSA) and internuclear dipolar coupling have a substantial influence on the behavior of a system of nuclear spins leading to a line-broadening effect in NMR spectra.
  • In order to overcome the problem of line-broadening in the solid state, magic angle spinning (MAS) NMR is applied. In MAS NMR, a sample is rotated rapidly around an axis at the magic angle with the static field yielding resulting averaging of all anisotropic interactions described by second-rank tensors, if the rotation frequency exceeds the largest coupling of the spin species considered.
  • Cross-polarization (CP) is used to assist in observing dilute spins, though it can also be used to perform some spectral editing and to obtain information on what spins are close in space. In CP pulse sequence the dilute X nucleus derives its magnetization from a nearby network of abundant spins. The key to obtaining efficient cross-polarization is meeting the Hartmann-Hahn condition. In this case the rf field of the dilute spins is set equal to that of the abundant spins by adjusting the power on each of the channels. If they are set properly, the abundant and dilute spins precess in the rotating frame at the same rate, allowing for the transfer of the abundant spin polarization to the dilute one.
  • The investigation of many physiologically and pharmaceutically active materials in the solid state is important, since their molecular and physicochemical properties in this state are directly related to their activities. Among several techniques available for the purpose, solid state NMR possesses some incomparable properties. For example, amorphous materials and heterogeneous systems can be readily studied, and polymorphs identified by inspection of the spectra. Moreover, solvates can be recognized, whether they are stoichiometric or not.
  • In addition to the basic concepts related to solid state NMR, during this mini-course detailed solid state studies of some pharmacologically interesting steroid derivatives will be described.
Language of instruction
English
Further comments (probably available only in Czech)
The course is taught only once.
The course is taught: in blocks.
Note related to how often the course is taught: 28.4. - 29.4. A4/0.57.
  • Enrolment Statistics (recent)
  • Permalink: https://is.muni.cz/course/sci/spring2016/IC151