Laboratory NMR

 


 

Head:
Karol Pasternak, PhD

 

 


 

Staff:

Anna Teubert, MSc

 

 


 
   
 

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Key words:

high resolution NMR spectroscopy, 1H, 13C, 31P, 19F, 29Si nuclei, one- and multidimensional (correlation) spectra, homo- and heteronuclear spectra, temperature experiments, automated spectra acquisition, material characterization, structure and dynamics of nucleic acids, CD and UV-vis spectroscopy, HPLC

 

Offer:

  • High-throughput and automated acquisition of 1D, 2D NMR spectra (for example COSY, HSQC, HMBC, NOESY, TOCSY)
  • Application of spectroscopic techniques such as NMR, UV-VIS, CD, ORD for structure determination of nucleic acids, study of ligand-RNA/DNA interaction.
  • Assessment of the nucleic acids purity based on HPLC, NMR, UV, CD.
  • Structure elucidation of organic compounds based on the analysis of 1D and 2D NMR spectra.
  • Acquisition and analysis of NMR spectra of multicomponent samples of natural origin i.e. herbal extracts, lyophilisate of body fluids, cell lisates.
  • Expertise in the interpretation of NMR spectra. Conformational study of natural or synthetic organic compounds.
  • Spectroscopic study of intra- and intermolecular interactions.

 

Equipment:

 

400 MHz (9.39 T) NMR Spectrometer AVANCE II Bruker

  • two RF channels
  • BBFO probe Z-gradient, 5mm – double resonance broadband probe optimized for X-nuclei detection. The inner coil is tunable over a frequency range that enables observation of nuclei between 97Mo and 31P, and 19F. The outer coil is optimized for 1H decoupling and observation. Temperature range: -80 oC to +130 oC.
  • BBI probe, H-BB, Z-gradient, 5 mm - double resonance broadband inverse probe optimized for 1H detection. The outer coil is tuneable over a frequency range that permits decoupling of nuclei between 109Ag-31P. This probe is used for experiments like HSQC, HMQC, and HMBC. Temperature range:-150 oC to +180 oC.
  • Automatic Tuning and Matching system
  • Automatic shimming system TOPSHIM

 

500 MHz (11.74 T) NMR Spectrometer AVANCE III Bruker

  • three RF channels
  • BBO probe, 1H-19F,(31P-15N)+19F,D, Z-gradient, 5 mm - double resonance broadband probe optimized for X-nuclei detection. The inner coil is tunable over a frequency range that enables observation of nuclei between 97Mo and 31P, and 19F. The outer coil is optimized for 1H decoupling and observation. This probe also enable recording of 1H-{19F}, 19F-{1H} and X-{19F}, 19F-{X} correlation experiments. Temperature range: -150oC to +150oC.
  • TXI probe, H-C/N,D, 5 mm, Z-gradient. Triple resonance inverse probe optimized for 1H detection with the outer coil tuneable for 13C or 15N. Triple Resonance Probe can be used to record triple resonance experiments of biological macromolecules labelled with 13C and 15N.

Temperature range: -150oC to +150oC.

  • Automatic Tuning and Matching system
  • Automatic shimming system TOPSHIM
  • The Bruker Automatic Sample Changer (B-ACS 120) together with IconNMR™ allows fully automated acquisition and processing.

 

700 MHz (16.44 T) NMR Spectrometer AVANCE III Bruker

  • Four RF channels
  • QCI-P probe, 1H/13C/15N/31P, 5 mm, Z-gradient- Quadruple Resonance CryoProbeTM - a proton-optimized quadruple resonance NMR inverse probe - increases sensitivity about four times on 1H and 13C compared to a room temperature QXI probe. Four fully independent channels of this probe enable simultaneous decoupling on multiple nuclei such as 13C, 31P and 15N. It is ideally suited to the study of RNA/ DNA and proteins, whilst also enabling research on small molecules and metabolomic samples. Temperature range: 0oC to +80oC
  • BBO probe, BB-H-D, 5 mm, Z-gradient -double resonance broadband probe optimized for X-nuclei detection. The inner coil is tunable over a frequency range that enables observation of nuclei between 97Mo and 31P, and 19F. The outer coil is optimized for 1H decoupling and observation. Temperature range: -150oC to +150oC.
  • TXI probe, H-C/N,D, 5 mm, Z-gradient
  • TXI probe, H-P/C,D, 5 mm, Z-gradient
  • Triple resonance inverse probes optimized for 1H detection while the outer coils are tuneable for 13C and 15N or 13C and 31P. Triple Resonance Probes can be used to record triple resonance experiments of proteins and nucleic acids labelled with 13C and 15N. Temperature range: -150oC to +150oC.
  • Automatic Tuning and Matching system
  • TOPSHIM Automatic shimming system TOPSHIM
  • SampleCaseTM is fully automated 24 sample changer that together with IconNMR™ allows fully automated acquisition and processing.

 

Spectropolarimiter circular dichroism (CD) Jasco J-815 S

J-815 is a Circular Dichroism (CD) spectropolarimiter from JASCO. The system is designed to measure CD in UV/Vis region but it has many optionally available measurement modes such as measurement of optical rotatory dispersion (ORD), linear dichroism (LD) or fluorescence.

Hardware Specifications

• Wavelength range CD: 180-900 nm

• Wavelength range ORD: 190- 600 nm, range of angle of rotation +/-35°

• Wavelength range LD: 200-800 nm

• Wavelength range for fluorescence emission measurement: 200-800 nm

Accessories:

Pelitier temperature control.

Automated Titration System that allows long term kinetic, chemical denaturation, and ligand binding studies.

Bio-Logic: SFM-20; two channel stop-flow setup.

 

Spectrophotometer UV VIS Jasco V-650

Double beam UV VIS spectrophotometer working in wide range of wavelength (190-900 nm) with a single monochromator and photomultiplier tube detector. Enables accurate measurements of low concentration samples with excellent linearity up to an absorbance of 4. Graphical user interface is available including Spectra ManagerTM II software that allow full system control and advanced data processing. Accessories such as automated cell changers and programmable temperature control systems allow full control by the Spectra Manager II.

Hardware Specifications

  • Wavelength range: 190-900 nm
  • Wavelength repeatability: 0.05 nm
  • Wavelength accuracy: ±0.2 nm
  • Spectral bandwidth: 0.1, 0.2, 0.5, 1, 2, 5, 10 nm
  • Scanning speed: 10-4000 nm/min
  • Photometric range: up to +4 Abs
  • Photometric accuracy: 0.002 Abs at 0-0.5 Abs
  • Baseline stability: ± 0.0003 ABS/h

 

Spectrophotometer UV VIS Beckman DU-640

The DU-640 Spectrophotometer is a microprocessor controlled single-beam spectrophotometer intended for use in quantitative and qualitative biological research. The instrument has three standard routine measurement modes including: Fixed Wavelength, Wavelength Scan, kinetics/time.

Hardware Specifications

• Wavelength range: 190-1100 nm

• Wavelength repeatability: 0.1 nm

• Wavelength accuracy: ±0.2 nm

• Spectral bandwidth: ≤ 1.8 nm

• Scanning speed: 120, 240, 600, 1200, 2400 nm/min

• Photometric range: up to +3 Abs

• Photometric accuracy: 0.005 Abs przy 1.0 Abs

• Baseline stability: ± 0.003 ABS/h

 

High Performance Liquid Chromatography system Agilent Tech 1260 Infinity

The system is equipped with variable volume autosampler, thermostated column compartment, diode-array detector, multiple wavelength detector, fluorescence detector, fraction collector, degasser and automatic purge valve integrated into pump module.

 

Selected publications from the last three years:

1. Stefański T., Mikstacka R., Kurczab R., Dutkiewicz Z., Kucińska M., Murias M., Zielińska-Przyjemska M., Cichocki M., Teubert A., Kaczmarek M., Hogendorf A., Sobiak S.
Design, synthesis, and biological evaluation of novel combretastatin A-4 thio derivatives as microtubule targeting agents.
European Journal of Medicinal Chemistry, 2018, 144, 797-816.

2. Długaszewska J., Szczółko W., Koczorowski T., Skupin-Mrugalska P., Teubert A., Konopka K., Kucińska M., Murias M., Düzgüneş N., Mielcarek J., Goślinski T.
Antimicrobial and anticancer photodynamic activity of a phthalocyanine photosensitizer with N-methyl morpholiniumethoxy substituents in non-peripheral positions,
Journal of Inorganic Biochemistry, 2017, 172, 67-79.

3. Wierzchowski M., Dutkiewicz Z., Gielara-Korzańska A., Korzański A., Teubert A., Teżyk A., Stefański T., Baer-Dubowska W., Mikstacka R.
Synthesis, biological evaluation and docking studies of trans-stilbene methylthio derivatives as cytochromes P450 family 1 inhibitors.
Chem Biol Drug Des. 2017, 90(6), 1226-1236.

4. Koczorowski T., Szczółko W., Burda K., Nowak M., Dawidowska M., Teubert A., Sobotta L., Gdaniec M., Korecki J., Mielcarek J., Tykarska E., Goślinski T.
Influence of bulky pyrrolyl substitent on the physicochemical properties of porphyrazines.
Dyes and Pigments, 2015, 112,  138-144.

5. Kryjewski M., Tykarska E., Rebis T., Długaszewska J., Ratajczak M., Teubert A., Gapiński J., Patkowski A., Piskorz J., Milczarek G., Gdaniec M., Goślinski T., Mielcarek J.
Porphyrazine with bulky 2-(1-adamantyl)-5-phenylpyrrol-1-yl periphery tuning its spectral and electrochemical properties,
Polyhedron, 2015, 98, 217-223.

6. Kucińska M.,  Skupin-Mrugalska P., Szczółko W., Sobotta Ł., Sciepura M., Tykarska E., Wierzchowski M., Teubert A., Fedoruk-Wyszomirska A., Wyszko E., Gdaniec M., Kaczmarek M., Goślinski T., Mielcarek J., 
Murias M. Phthalocyanine Derivatives Possessing 2-(Morpholin-4-yl)ethoxy Groups As Potential Agents for Photodynamic Therapy.
Journal of Medicinal Chemistry, 2015, 58 (5), 2240-2255.

7. Stefański T., Mikstacka R., Kurczab R., Dutkiewicz Z., Kucińska M., Murias M., Zielińska-Przyjemska M., Cichocki M., Teubert A., Kaczmarek M., Hogendorf A., Sobiak S.
Design, synthesis, and biological evaluation of novel combretastatin A-4 thio derivatives as microtubule targeting agents.
European Journal of Medicinal Chemistry, 2018, 144, 797-816.

8. Długaszewska J., Szczółko W., Koczorowski T., Skupin-Mrugalska P., Teubert A., Konopka K., Kucińska M., Murias M., Düzgüneş N., Mielcarek J., Goślinski T.
Antimicrobial and anticancer photodynamic activity of a phthalocyanine photosensitizer with N-methyl morpholiniumethoxy substituents in non-peripheral positions,
Journal of Inorganic Biochemistry, 2017, 172, 67-79.

9. Wierzchowski M., Dutkiewicz Z., Gielara-Korzańska A., Korzański A., Teubert A., Teżyk A., Stefański T., Baer-Dubowska W., Mikstacka R.
Synthesis, biological evaluation and docking studies of trans-stilbene methylthio derivatives as cytochromes P450 family 1 inhibitors.
Chem Biol Drug Des. 2017, 90(6), 1226-1236.

10. Koczorowski T., Szczółko W., Burda K., Nowak M., Dawidowska M., Teubert A., Sobotta L., Gdaniec M., Korecki J., Mielcarek J., Tykarska E.,
Goślinski T. Influence of bulky pyrrolyl substitent on the physicochemical properties of porphyrazines.
Dyes and Pigments, 2015, 112,  138-144.

11. Kryjewski M., Tykarska E., Rebis T., Długaszewska J., Ratajczak M., Teubert A., Gapiński J., Patkowski A., Piskorz J., Milczarek G., Gdaniec M., Goślinski T.,
Mielcarek J. Porphyrazine with bulky 2-(1-adamantyl)-5-phenylpyrrol-1-yl periphery tuning its spectral and electrochemical properties,
Polyhedron, 2015, 98, 217-223.

12. Kucińska M.,  Skupin-Mrugalska P., Szczółko W., Sobotta Ł., Sciepura M., Tykarska E., Wierzchowski M., Teubert A., Fedoruk-Wyszomirska A., Wyszko E., Gdaniec M., Kaczmarek M., Goślinski T., Mielcarek J.,  Murias M.
Derivatives Possessing 2-(Morpholin-4-yl)ethoxy Groups As Potential Agents for Photodynamic Therapy.
Journal of Medicinal Chemistry, 2015, 58 (5), 2240-2255.