Derivatization with MTBSTFA / problem
Posted: Tue Jan 20, 2026 5:32 pm
Hi, I would like to ask for your opinion.
Why does my derivatization reaction with MTBSTFA not seem to proceed? I do not see any difference between the blank and a high-concentration standard.
At the moment, I am running the experiment using only neat standards of phenols and glycols. My procedure is as follows:
50 µL of the standard in LC–MS grade acetonitrile (water ≤ 0.01%),
50 µL of acetonitrile,
50 µL of MTBSTFA,
heated at 80 °C for 60 min,
cooled to room temperature,
then 1000 µL of n-hexane (FID/ECD grade) is added.
I collect the upper hexane layer and analyze it by GC–MS. The blank is prepared in the same way.
I do not observe any peaks corresponding to the phenols or glycols, despite the high concentration.
Why does my derivatization reaction with MTBSTFA not seem to proceed? I do not see any difference between the blank and a high-concentration standard.
At the moment, I am running the experiment using only neat standards of phenols and glycols. My procedure is as follows:
50 µL of the standard in LC–MS grade acetonitrile (water ≤ 0.01%),
50 µL of acetonitrile,
50 µL of MTBSTFA,
heated at 80 °C for 60 min,
cooled to room temperature,
then 1000 µL of n-hexane (FID/ECD grade) is added.
I collect the upper hexane layer and analyze it by GC–MS. The blank is prepared in the same way.
I do not observe any peaks corresponding to the phenols or glycols, despite the high concentration.