HMDS-fatty acids
Posted: Thu Apr 17, 2014 9:04 am
by GCrF
Dear all,
can someone suggest me a sylation protocol using the HMDS reagent?
Many thanks
Re: HMDS-fatty acids
Posted: Thu Apr 17, 2014 1:05 pm
by MSCHemist
Are we talking short chain fatty acids? Otherwise most labs do FAMES. I prefer chloroformates over silytating reagents since they are not water sensitive and don't foul up the instrument.
http://onlinelibrary.wiley.com/doi/10.1 ... 3/abstract
Re: HMDS-fatty acids
Posted: Thu Apr 17, 2014 2:01 pm
by GCrF
with FAMEs method I've some difficulties to detect hydroxy-F.A. I'm interested on C-12 to 18.
Re: HMDS-fatty acids
Posted: Thu Apr 17, 2014 3:00 pm
by MSCHemist
HMDS is a rather weak agent.
From Handbook of Analytical Derivitizations
Dissolve in HMDS/TMCS/pyridine 2:1:10 add 2.5 molar equivalents BSA in pyridine and incubate at RT for 2 hours
or
dissolve in 50ul BSTFA, 50ul Pyridine heat to 50-60 deg for several hours [I'd imagine inlcuding 1% TMCS would help]