Unexpected fragmentation

Chromatography Forum: LC-MS & GC-MS Archives: Unexpected fragmentation
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Andreas on Saturday, June 22, 2002 - 02:07 am:

We are conducting fatty acid analysis using MTBSTFA derivatization. Usually for such derivatives the most abandoned ion is m/z=M-57 - fragment resulting from the elimination of tert.butyl group. In our case this is true for dicarboxylic acid,but not for monocarboxylic. For monocarboxylic fatty acid the main fragment ion is m/z=M-39 or in other words m/z=M-57+18.
If anybody can explain this anusual (at least for me) fragmentation pattern?
If this is water adduction, why not for dicarboxylic acid?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Molever on Monday, June 24, 2002 - 04:19 pm:

I'm in the soap industry, and we have experience with fatty acid and derivatives. I tried pure myristic acid with MTBSTFA (we've used BSTFA before). With BSTFA I get trimethylsilyl derivative MW peak at 300 (228.4 + 73 -1 for hydrogen) and a larger (largest) peak at M/z 285, corresponding to a loss of a CH3 methyl group (MW-15). With MTBSTFA, I don't get a peak at M/z 300, just the large M/z at 285 (still) which corresponds to the MTBSTFA derivatized MW of 342.6 less 57 (loss of t-butyl group). I didn't see any MW-39 at all.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Andreas on Wednesday, June 26, 2002 - 04:43 am:

Molever, can I ask what MS do you use - quadrupole or ion trap?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Molever on Wednesday, June 26, 2002 - 08:25 am:

We have quadrupole (HP 5971A and 5972A). I just reprepared and reinjected Monday, for you.


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