sample cleanup for GC-MSD

Discussions about sample preparation: extraction, cleanup, derivatization, etc.

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Interested in sample clean-up for GC-MSD analysis of short chain fatty acids in background media. The background may contain moderate levels of proteins and sugars. Would like to cleanup as much as possible up-front. Methods suggested: initial organic extraction (protein cleanup) followed by HILIC SPE for binding sugars.
Would really like hear your comments on this, plus other methods that you have tried or feel may be a better option.

Thanks for your help.
It depends on your sensitivity needs but I like doing total evaporative headspace esterification. No cleanup necessary

into a 10ml headspace tube
2.5ul concentrated sulfuric acid
2.5ul sample (use a branched acid as itsd like 4 methyl pentanoic)
5ul alcohol of choice to esterfy with methanol ethanol propanol isobutanol
incubate the tube at 120degC for 60 min

I sample 2ml headspace 5:1 split. and get nice clean esters. It works with lactic, succinic, and fumaric as well.
2 posts Page 1 of 1

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