Hi researchers,
I need to analyze acrylamide in food samples by using GC-MS. Prior to the GC-MS analysis, I performed a derivatization step using silylation agent. I tried BSTFA + 1% TMCS to derivatize acrylamide, but I failed to get a satisfactory outcomes. At first I tried to derivatize acrylamide by spiking 100 uL of BSTFA + 1% TMCS into a 500 uL of acrylamide (at known concentration) in ACN. Subsequently, I incubate the mixture at 70 degree celcius for 1 hour and injected the aliquot into the GC-MS. Unfortunately, no peak was detected at the observed m/z ion. I also tried to increase the volume of BSFTA use from 100uL to 250uL, but it still does not works. Please help me, I am literally clueless on how to solve this conundrum.
Have you checked the suggestions of firms like WATERS, see for example https://blog.waters.com/is-burnt-toast-safe-how-do-food-testing-labs-find-acrylamide
Dear,
ACN it is not a proper solvent for silylation because it has water!! And Water react with MSTFA/BSTFA consuming the derivatization mixture.
Chance your solvent and the rest it is OK.
best regards
Eleuterio
Hi Elutereo, based on various silylation method with MSTFA/BSTFA used ACN. The ACN used in my research is 99% purity. Hence, I believe water in ACN is not an issue.
Dear Naziruddin
ACN form an azetrope with water, so only ACN 99% anhydrous it is useful for silylation. Just to check that information because normally bad derivatization implies the present of water or alcohol or traces of acids in the solvent.
By the way in your title said MSTFA/BSTFA but in the explanation you only give information for BSTFA + 1% TMCS.
Are you looking for N,O-Bis(trimethylsilyl)acrylamide? or N,2-Bis(trimethylsilyl)acrylamide
Best,
https://assets.thermofisher.com/TFS-Assets/CMD/posters/po-90518-gc-ms-acrylamide-food-rafa2019-po90518-en.pdf
- Badges
- Science topic
- Similar topics
- Philosophy
- Esthetics
- Interpretation