3-hydroxypropionaldehyde analysis by GC-FID

[cay1000]

hi all,

I would like to quantify 3-hydroxypropionaldehyde (3-HPA) by GC-FID.

First of all,the sample is containing 3-HPA in phosphate buffer (& KCl). Here, I am wondering how to inject samples properly. (NO autosampler available, so manual injection only)
Do I need a sample treatment such as extraction? I would like to try SPME, but I do not have experience SPME manual injection.
Currently, the equipment(agilent) was installed with HP-1 column and FID.
Help me, please!

Thanks,

Kelly

[Don_Hilton]

The best procedure for keeping the GC inlet clean would be extraction of the analyte from water. But 3-hydroxypropionaldehyde may be a bit difficult to extract. I note the following:
http://www.sciencedirect.com/science/ar ... 7X12000583, which has a complex matrix, but puts the liquid from a cell culture into the GC inlet, dilited with acetonitrile.

Look around and see what others have done. If there is a way to eliminate or reuce the salts and water before injection, it would be better.

[MSCHemist]

SPME can have issues when used for quantitation especially manually. You would need a really good ITSD. You might want to consider drying the sample and derivitizing with BSTFA. Otherwise you may have some sucess salting it out of water into ethyl acetate or even acetonitrile (with enough salt it forms a separate layer from water) however it is such a small polar compound you may need to use a thick phase wax column or cyanopropyl column or it could come out in the solvent peak or have poor peak shape.

I think with SPME and a db-1 column you would see very poor peak shape as it would be a very small polar compound with no affinity for a nonpolar db-1 column and it could also be tough to focus as it takes a minute to desorb off the fiber.

[bunnahabhain]

You might want to consider drying the sample and derivitizing with BSTFA

May I just jump in here: Is it possible to do this derivatisation in aqueous solution?
joerg

[MSCHemist]

No almost all derivatizing agents are sensitive (rapid hydrolysis of both the reagent and product) to water as well as other protic solvents such as methanol, ethanol, isopropanol. All the silylating agents in particular are. The usual procedure would be to dry it and redissolve in pyridine, acetonitrile, DMSO, DMF, or actually the reagents themselves.

The only derivatizing reagents commonly used that aren't water sensitive are the alkyl chloroformates which I use a lot but won't derivatize an aliphatic alcohol nor aldehyde group.