Recently, I have tried to set up the 15N INEPT pulse program (ineptrd and
ineptpnd) in Bruker for methyl anthranilate which has an NH2 group, a
standard sample used by Bruker. Unfortunately, it does not work. However, I
tried both HMBC and an inverse gated pulse program (N15IG in parameter set)
for it. Both worked in our 600 and 400 MHz BBFO probe as shown in the
below. The HMBC took 1.5 hrs (even 20 min can get a nice spectrum) and the
zgig took 3 hrs at 600 MHz. I also tried HSQC for the above compound which
does not work, possibly due to the fast H exchange of NH2 group. However,
HSQC works for Gromicidine in DMSO.
On Wed, Apr 2, 2025 at 11:27 AM Qi Wu via groups.io wrote:
> Hi Dr. Gemmecker,
>
> I have some related questions on 15N. I have Bruker and PA BBO probe (with
> X on the inner coil I assume). I'm looking to quantify levels of primary,
> secondary and tertiary amine for polyamine (aliphatic) and its reaction
> products. I've tried the standard 1H-15N 2D NMR experiments, but the HSQC
> didn't work well, and got some data from HMBC.
> Do you have any suggestions for 2D to assign the various amines (Bruker
> preset experiments, pulse programs, parameters)?
> Also if 2D is not quantitative, is it reliable to quantify 1, 2 amines
> using 1H with the labile Hs, and using solvents such as DMSO and acetone?
>
> Thank you and best regards,
> Qi
>
>
>
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Received on Thu Apr 03 2025 - 05:47:41 MST