I would like to do disodium guanylate (GMP) and disodium inosinate (IMP) via GC. I have tried 6 different reagents and dozens of conditions and none has been successful despite publication indicating it should work. I've tried methyl and ethyl chloroformate, phenylboronic acid for the ribose diol followed by the chloroformates, BSTFA + TMCS, MSTFA + TMCS and on column alkylation with phenyltrimethylammonium hydroxide. No luck. Does anyone have a protocol that works? Most of the papers I've seen date back to the 70's there was a recent report that NAD+ and NADP+ work with methyl chloroformate but as I said it didn't work for me.
Dear Steven, I doubt that you get these guys over a GC column. The only suggestion I have is try to cleave the phosphate group before derivatisation. Even then I would not be too surprised it does not work. the sugar alone and the basic ring alone have a good chance. That is probably what happened in the old literature. The other option is use HPLC.
I finally got silylation working. Inosinate was clearly visable and made a good peak after silylation with MSTFA+TMCS in pyridine after microwaving. Guanylate though had a much lower response and a blob that fronts up to it with different m/z ions indicating it is probably decomposing in the GC.
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