Problem with the analysis of 3-MCPD

[cheebeng]

Dear all,

I am currently working on the analysis of 3-MCPD using GCMS.

According to the published method of analysis, the method requires derivatization of 3-MCPD with phenyl boronic acid.

Does anyone of you have any experience before on the derivatization of 3-MCPD? My sample is 3-MCPD standard alone in ethyl acetate at concentration about 0.5-1ppm, kindly share with me the simple way how to derivatize the compound.

Thank you

[klfarris]

would suggest that you contact the authors of the paper you are following

[MSCHemist]

What a coincidence I just started a new position and 3-MCPD is one of our major tests. Our method uses diamtomaceos earth columns (EMD ChemElut) and heptafluourobutylimidazole for derivitization.

[MSCHemist]

It is a tricky analysis. In our method we take 3g of solid sample + 9g water and add 2.5ml of sample to Agilent Chem Elute cartridges X2 for a total of 5ml of sample and 2 cartridges. We elute each cartridge with 2X5ml of ethyl acetate for a total of 20ml from 2 columns. We then blow it down to 1 ml with N2. Then we add 4ml of hexanes and 100ul of hfbi and 0.5 ml of 20ppm MePD ITSD and react for 15 min. Then we blow it down to 1ml again and shoot 2ul splitless.

added after reacting we extract with water 3 times and discard the aqueous layer to remove HFBI and add sodium sulfate to remove resisdual water.

[MSCHemist]

Has anyone seen a method using hydrogen as a carrier? This is one of our big tests and I've never seen an H2 carrier method for it.

[MSCHemist]

I've been busy for the past month fixing our 3-mcpd method. Basically our old method had SPE recovery problems, dilution factor calculation errors and chromatography issues pretty much the holy trinity of method fail.

I've fixed the recovery issues, the dilution calculation issues, and the peak shape issues. Our method is based of derivitization with HFBI. I have just started experiementing with phenyl boric acid and am waiting for a new internal standard. Our HFBI method uses 3-methoxy 1,2 propane diol at the ITSD. I can't resolve it from 3-mcpd using the PBA method so I am going to try propane 1,3 diol or ethylene glycol.

The last remaining issue I am having is we have never been able to achieve resolution between 3-mcpd-HFBIderivative and 2-mcpd-HFBIderivative. Like most other publications and the AOAC method we use a 30m .25mm .25um DB-5ms column and we've tried columns from 5 different manufacturers over the years with no difference. We get almost resolution on some samples and little resolution on others bases on the ratio of 2 to 3 mcpd present.

Is anyone here working on this analysis. It has been reported a Innowax column works but it is very vulnerable to attack by residual HFBI. Has anyone tried a higher phenyl or cyanopropyl column?