Gluteraldehyde by MS

[James_Ball]

I am working on a project to analyze gluteraldehyde in process water in a paper plant and am wondering what options I have for analysis. Normally I would just derivatize with DNPH and use HPLC/UV, but I am wondering if it is possible by purge and trap GCMS underivatized or maybe GCMS with just C18 SPE and concentration in Acetonitrile or Ethylacetate with direct injection.

Ketones I know chromatagraph well but is there a chromatographic reason for derivatizing aldehydes, other than to make a larger molecule? The mass of gluteraldehyde is large enough to be detected by MS so if it will give a good peak it should work, but it is one I have never tried before. Has anyone had any experience with this analysis?

[Consumer Products Guy]

Has anyone had any experience with this analysis?

Sometimes it seems that I have hands-on experience with just about everything !

We've assayed for glutaraldehyde (that's the correct spelling, by the way) using GC in the past, dissolved samples in water and direct GC, polar column. I've never tried by headspace or used the GCMS for glutaraldehyde though.

We've also used 2,4-DNPH derivatization and HPLC, and that worked well too.

[Peter Apps]

I doubt that it will work by headspace, except perhaps with complete evaporation. I ran sterilants that contained ethanol and glutaraldehyde by HS, and there was no sign of any peak apart form the ethanol.

Peter

[James_Ball]

Thanks everyone!

I had my doubts about purge and trap, even though we have had samples that showed hits for acetaldehyde before, but it was extremely high in the sample. The client is looking for levels at 0.5-1ppm so I may give it a try and see if I can recover some if I elevate the temperature, but I don't look to get a really big response, and will probably not give a good peak on a Rtx624 column.

I will definitely give it a try on the FID with Wax column since the detection limits required are so high, if I can't see it there then I know the DNPH/HPLC will work.

[MSCHemist]

http://www.ncbi.nlm.nih.gov/pubmed/12061557
http://www.sigmaaldrich.com/technical-d ... iable.html