GPC PCB clean-up

Record: 874

Category: Applications
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Question
I was wondering if you could help me with an application I am currently developing for the clean-up of PCBs in dairy products as requested by one of our local customers prior to GCMS. I have purchased a EV-200 for small scale clean-up (to be collected into 1.5ml vials) and have two marker PCBs upper/lower to determine the collection start/stop times. I was wondering if you already had some optimised conditions for this type of application. I was also wondering what impact using ethylacetate or acetone makes to the separation, is this related to the analyte solubility only or the pore size of the column particles? I will need to use the former as acetone absorbs up to 330nm which would make detecting the marker pcbs difficult for the initial set-up. The dairy will be extracted into an organic solvent probably cyclohexane prior to GPC.

Any help you can offer would be appreciated.

Answer
I do not have an application for PCB in dairy as requested, but I do have some information that may help.

The column solvent for EV-200 is shipped with ethyl acetate/cyclohexane 30/70, but the solvent may be replaced with acetone/cyclohexane. See the operation manual attached. The larger dimension columns EV-2000 and EV-2000 AC are identical in packing material to your EV-200 except for the in-column solvent. So I think that the different solvents are more useful for the solubility of the target compounds and the retention of the compounds rather than have any effect on the packing material.

For the analyses using acetone our tech support used a UV cutoff filter and changed the optical pass length inside the detector because acetone has a large absorbance until 330 nm. RI detection could also be used; however, you may not want to change the detection method. Do you have access to a UV cutoff filter?

Here is the elution profile for pesticides using EV-2000 AC with acetone/cyclohexane:
http://www.shodex.net/index.php?seitenid=1&applic=923

However, I have not found a similar table for the elution using ethyl acetate/cyclohexane.

Please let me know what compounds you are using for your upper/lower markers, and I may be able to find more information.

 
 
Additional Comments
I just noticed that you are contacting me from Australia. You might have a faster response from our tech support in Japan. I am located in the US, and so our time difference will make the email communication take longer especially if I have to check with tech support to find additional information.

Here is the link to contact Shodex in Japan:
https://www.shodex.com/inquiry/f01e.html?pagetitle=Shodex+English+Top

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