I am working with thermal desorption gas chromatography-mass spectrometry (TD-GC/MS) and need to derivatize organic compounds before analysis. However, I am unsure about the best approach for performing derivatization when loading samples onto an empty glass tube.
Could anyone share standard protocols, recommended reagents, or practical tips for ensuring effective derivatization in this setup? Any insights or references would be greatly appreciated.
Thank you in advance for your help!
Key Derivatization Techniques
Silylation (using BSTFA, MTBSTFA, TMSI) is optimal for functional groups such as -OH, -COOH, and -NH.
Acylation (employing TFAA, PFPA, HFBA) enhances the detection of amines and phenols, making it suitable for electron capture detection (ECD) and negative chemical ionization mass spectrometry (NCI-MS).
Alkylation (via Diazomethane, TMAH) facilitates the transformation of carboxylic acids into esters.
Essential Recommendations
Minimize the amount of reagent used to prevent contamination.
If reactions on the tube are unsuccessful, consider pre-derivatizing in solution.
Conduct reagent blanks to identify any potential artifacts.
For derivatives that are sensitive to heat, lower the thermal desorption temperature.
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