Epichlorhydrin by GC MS

[Fr]

I'm trying to develop a method by GC (MS or FID) for epichlorhydrin in API but epichlorhydrin isn't really stabile. An idea?

[chromatographer1]

I developed a headspace method to measure epichlorhydrin at less than 1 ppm several years ago and was able to detect less than 0.25ppm and to linearly add up to 5ppm in sample spikes.

It is a difficult analysis if excessive heating is used.

Sorry but I cannot share the details of the analysis.

[Fr]

Ok, so the fact I'm trying and not really succeed in something is quite consistent. I've noticed that headspace wasn't easy to use for that because of the instability of epichlorhydrin when heating it (and the matrix I use (benzyl alcohol) is unsuitable also. I understand that you can't share anything but can't you orientate me?

[chromatographer1]

I suspect there is something in your matrix that might be reacting with the epichlorhydrin.

The column used was a moderate polarity cyanopropyl phenyl phase and the API matrix was a water solution of the API at a high concentration. No bare metal surfaces contacted the sample. Heating was kept at less than 85°C for a period of less than 15 minutes. There were lots of other peaks at 1ppm levels which we dodged by adjusting the temperature of the column so the ECH eluted without an interference. Teflon coated vial cap septa were used.

Salt and absence of salt made little difference of the recovery of ECH.

A Varian Genesis HS analyzer was used. (also known as a Tekmar 7000)

[Fr]

thanks for all those tips, I'm trying that soon.