High throughput measurement combining No-D NMR and NUS

  • Summary

NM180016E

No-D NMR is a method to obtain high resolution 1H spectrum without deuterated solvents. It suggests that any reaction mixture or reagent solution are directly available for No-D NMR measurement. Although a huge proton signal of non-deuterated solvent is observed, it could be suppressed by using WET sequence.
On the other hand, since No-D NMR doesn't use NMR LOCK, chemical shift gradually changes during long time experiment. As a result, the line width of NMR signals become broad for long time experiment. Therefore long time experiments (such as 2D measurement) would make less quality data in No-D NMR.
In this note, measurement of high resolution 2D NMR spectra in No-D NMR by combining NUS(Non-Uniform Sampling) is introduced.

Our No-D NMR automation detects and suppresses solvent signals automatically, therefore no need for these messy operations manually. These optimization function can be applied not only to 1D NMR but also to 2D NMR. Therefore multiple 2D experiments can be set continuously without selecting solvent signals and setting the solvent's chemical shift manually.

Fig.1 spectra show high resolution NMR spectrum observed by No-D NMR.
Fig.2.3.4 show general 2D NMR spectra using solvent suppression and NUS. Correlation signals could be observed despite of short measurement time.

Fig.1:  Top:1H , Bottom :No-D ext time: 1min(※ solvent signal)
Fig.1: Top:1H , Bottom :No-D ext time: 1min
(※ solvent signal)
Fig.2:  COSY(NUS25%)  ext time: 4min
Fig.2:  COSY(NUS25%)  ext time: 4min
 
Fig.3:  Edited HSQC(NUS25%)  ext time: 15min
Fig.3:  Edited HSQC(NUS25%)  ext time: 15min
 
Fig.4:  HMBC (NUS25%)  spectrum , experiment time: 9min
Fig.4:  HMBC (NUS25%)  spectrum , experiment time: 9min
 

Sample:5mg rotenone/ acetone
Console:JNM-ECZ400S

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