I want to use gas chromatography to analyze substances containing amino group, but because of the strong polarity of amino group, it may damage the chromatographic column, so i need to derivate it first. I have tried to use MSTFA and ECF for derivatization, but the former is not effective, and the latter is a dangerous and it cannot be purchased. Have anyone done similar experiments before? Or maybe you could help me find another way to derivate.
I would definitely do a TMS silylation. Using a molar excess of e.g. BSTFA - perhaps with a catalyst like TMCS - in anhydrous pyridine at a slightly elevated temperature should do the trick. But there are tons of protocols for silylation out there. Keep in mind that silylation is not exclusively selective for famines.
Article [3] Gas-liquid chromatography (GLC) of amino acid derivatives
http://www.phmd.pl/api/files/view/29738.pdf
I agree with Simon! If you already have mstfa, you can use it, it definetely works. In the Link there is a detailed protocol as well as retention indices for the different derivates (supplement)
Good luck!
https://www.nature.com/articles/s41598-018-22073-7
I would also prefer silylation - keep in mind that water reacts with the silylation reagent, so the best is to evaporate the water prior to derivatization!
For Amino groups, the best derivatization method is sillylation. You can use a reagent like BSTFA in presence of dry pyridine at around 70 deg. The problem is your sample is aqueous in nature and your silylation reagent has a very high reactivity with water. So you will have use a large quantity of the reagent to get your compound silylated. If you can extract the compound from water using an organic solvent and then silylate, it will be good.
- Badges
- Science topic
- Similar topics
- Analytical Chemistry
- Column