Chromatography Forum

Hi,

i want to clean-up my material samples (rubber) to analyse 16 EPA + benzo(j)fl. + Benzo(e)pyrene by GC-MS. We have to measure very low concentrations (0.2 mg/kg per compound).

Does anyone know a clean up methode for the 18 PAH? I've tried several SPE clean-ups with SiOH but hadn't any success with that. Also LC-FLD and GC-MS/MS weren't useful to get a clean chromatogramm.

I read about a method based on two praparative LC-steps: clean up with silica column followed by a clean up with a column filled with sephadex LH-20. It sounds very time- and solvent-intense. Does anybody know this clean up method or have a good alternative?

Thanks!

Silver coated alumina works wonders. Also, you can try partitioning with DMSO.

I tried partitioning with DMF/H2O (9/1), also no effect.
Where can i find silver coatet alumina? Has it a special trade name?

Next i will try clean up with Bio Beads SX3 (polystyrene divinylbenzene copolymer). Maybe GPC will help out hear.

Hi,
Have you already tryed with Florisil?

How does your extraction procedure looks like so far?