3. For a quantitative study of slow motions by means of R1ρ, one has to sample the spectral density functions J(ω) at rather low frequencies. In the case of R1ρ experiments under MAS, the lowest sampling frequency is determined by the difference |ω1 − ωR|. Because of the hardware limitations for selleck products the upper ω1 value, one may easily adjust this difference to any desirable value only if the MAS frequency is not higher than 25–30 kHz. ω1 can be increased by using resonance offset of the spin-lock frequency [18]. In this
case, however, the relaxation becomes slower, which requires longer spin-lock pulses and practically this is not always feasible. At high MAS frequencies (>50 kHz) one cannot obtain low values of the difference |ω1 − ωR| and hence, effectively study slow motions. Thus, the moderate (10–30 kHz) MAS frequencies seem to be an optimal compromise between the spectral resolution (which for deuterated proteins is rather decent), and possibility to adjust spin-lock and MAS frequencies close to each other, if one aims at studying slow motions using R1ρ measurements. We have demonstrated that rotating-frame relaxation rates (R1ρ) measured in deuterated and partially proton back-exchanged proteins can be used for a quantitative analysis
of slow μs–ms conformational PD-0332991 clinical trial dynamics of proteins at all MAS rates. In the chosen example of the SH3 domain, an analysis Ureohydrolase of the integrated signal intensity reveals that slow dynamics is rather abundant in this small protein, and occurs mainly in residues that are not resolved in 2D spectra, i.e., too broad to be detected. Clearly, site-specific
dynamic information is much more valuable than the integral characterisation of protein motions. The prerequisite for the former is a high spectral resolution which is achievable only at (relatively) fast MAS. At the same time, one should be aware that the analysis of only well resolved sharp peaks in 2D spectrum in some cases may not provide a comprehensive picture of the slow protein mobility, stressing the diagnostic use of a comparison between an integral measure of R1ρ from a 1D spectrum and a corresponding average over the resolved signals in a 2D experiment. This work was funded by Deutsche Forschungsgemeinschaft (DFG, SFB-TRR 102 project A8) Rauf Kurbanov is thanked for useful discussions. “
“Eine Reihe von Spurenelementen und Mineralstoffen sind für eine Vielzahl von lebensnotwendigen, biochemischen Prozessen unbedingt notwendig – sie sind somit essentiell. Allerdings sind diese Spurenelemente für die belebte Natur häufig schwer zugänglich.