Chromatography Forum

Hello,

I am looking for some information/experiences on analyzing for DMF by HS-GC-FID. Searching the forum I found a few posts mentioning that there can be problems. Is it due to the boiling point of DMF, is it a "sticky" compound? Anyone have experience testing for DMF by headspace?

Thanks,
Dave

I had much more luck with methods where the API was dissolved in a solvent such as DMSO and a liquid injection method was used to detect DMF rather than headspace.

However something like DMI as a diluent might not be a bad starting point if you have no other option but to use headspace. I had no luck with it personally, but your mileage may vary.

This Agilent blurb shows how DMF holds up to other solvents in terms of FID detection limits.

https://www.agilent.com/cs/library/appl ... 9726EN.pdf

In spite of the fact that European Pharmacopoeia provides general HS-GC-FID method to determine among others DMFa & DMSO, our lab decided to develop and validate HPLC-UV methods for such residual solvents. GC-FID is fine too but liner usually degrades too fast.

I don't see DMF as a problem. My short look at it today tells me I'd try to use a wax phase if possible but I can see 35 ppm in a plasticized pvc material easily using spme.

https://1drv.ms/b/s!AkH-uI0tnY5Le9xJJRT0XkjQy7E