Chromatography Forum

Hi All,
I have to determine residual mono-ethanol amine in a active pharmaceutical ingredient at ppm level.
My API is only slightly water soluble and I have a lot of problem to obtain the desired sensibility.
I made tests with GC-FID with split injection but without succes.
Could you please give me some suggests?
Thanks in advance
GT

This is not an easy test to develop. GC may not be the best technique to use.

I would consider attempting to separate the EA by flash chromatography and to concentrate the extract to perform a limit test by TLC or LC.

I suspect while performing the test on a new column and inlet, any serious attempt to do this analysis by GC will be prone to failure quite easily.

Good luck,

Rod

I use GC to assay for MEA periodically, no problems, and nice peak shape. I do derivatize but unfortunately I cannot disclose any more due to proprietary concerns, sorry.

GT

CPG is not a beginner and has a lot of experience and knowledge. You could be challenged by trying to use GC.

MEA derivatization can be done within some matrices but not EASILY with others.

If you can isolate the ethanolamine through flash chromatography, then you might find derivatization easier to achieve.

Whether you use a TMS or an trifluroracetate derivative, it still requires an injection of the matrix unless you isolate the MEA first. This can stop you in your tracks with some matrices.

The real barrier here is the lack of information and only you can decide what you can properly disclose.

GOOD LUCK,

Rod

GT,

To steal Rodney's often used advice, contact the column vendors and ask what their views are. I know that Chrompack used to offer a column for ethanol amine analysis and I believe that Restek offers a trace amine column that might be suitable but until you can find an appropriate column you won't get very far. When faced with a new application that is always the place that I start.

Best regards,

AICMM