GC Derivatization

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Offline kumar11

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GC Derivatization
« on: 18/12/2013 03:16:40 »
I am planning a series of gas chromatography derivatization experiments using silylation reagents, MSTFA, BSTFA, TMSI and TMCS (as shown newbielink:http://www.covachem.com/silylation_reagents.html [nonactive]).  It is possible that I will also be exploring MTBSTFA as a GC derivatization reagent as well.  Prior to GC/MS analysis, I intend to derivatize a series of compounds with multiple derivatizable functional groups (amine, alcohol, and carboxylic acid), and I hope to develop a cocktail of reagents that will lend itself to complete derivatization with as mild of conditions as possible (meaning lower heat). 

I recall an article that I read years ago showing that mixing TMSI, BSTFA, and TMCS together can give a more complete derivatization than any one silylation reagent alone.  I am wondering if any experts out there may have any insight into this type of reagent mixture, or if there might be a review out there regarding this type of chemistry.  Thanks for any guidance provided.


Offline chiralSPO

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Re: GC Derivatization
« Reply #1 on: 18/12/2013 19:49:03 »
All of these reagents are trimethylsilylating agents. And, while some of them have different selectivity profiles, I'm not sure how beneficial the cocktail would be. My gut reaction is that anything that would react with TMCS would also react with TMSI. BSTFA is probably the most active of the list, and should silylate anything that the others would be able to do.

I will look for some references. Stay tuned!