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terpene pyrophosphates

Posted: Wed May 21, 2008 7:35 pm
by mardexis
Anybody have any experience working with these compounds? C5 thru c20 pyrophosphate?

The MS detection is pretty straightforward but the pyrophosphates don't seem to come through any of the silica columns that I have tried. I don't think they are retained on the C18 but are being adsorbed elsewhere. They also seem to tail really badly by FIA unless I take out every piece of stainless that I can. I also tried a H form ion-exclusion and they never came out with 0.005 M sulfuric mobile phase.

I'm looking for a method of separating c5, c10, c15 and c20 turpene pyrophosphates. Any experience or suggestions?

Thanks,
Marc

Posted: Wed May 21, 2008 7:57 pm
by Kostas Petritis
There have been previous publications that use LC (silica based columns) to separate these kind of compounds (i.e. Analytical Biochemistry Volume 336, Issue 1, 1 January 2005, Pages 51-59). You could try to passivate your HPLC with EDTA.Na in the same way I have described in one of my previous posts (the advantage of EDTA is that you can passivate your chromatographic column as well...

Posted: Fri May 23, 2008 1:37 am
by mardexis
Thanks Kostas,

The article you mentioned should be helpful. The authors were derivatizing the pyrophosphates (with a peptide) before analysis. Maybe this was for good reason.