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d4 furan losses during sample treatment

Posted: Thu Jun 22, 2017 2:32 pm
by CrisGM
Hello everyone!

I'm a master student and I'm doing my final project about detection of furan in coffee from vending machine through the GC-MS/ SPME method.

However, when I put the d4 - furan into the vial with the coffee sample, exposing it to the fiber and analyzing it into de chromatograph, the chromatogram shows me a very low value of the d4 furan (about 87 - 90% of losses) in comparison with the values detected when the standard straight line was made.

I've been looking for a solution in some papers, but I dont't find anything that helps me.

Does anyone know something about it?

Thank you!

Re: d4 furan losses during sample treatment

Posted: Thu Jun 22, 2017 3:57 pm
by Peter Apps
Welcome to the forum.

How did you do this bit " when the standard straight line was made." ? In detail please - the more you tell us the more we can help.

Peter

Re: d4 furan losses during sample treatment

Posted: Thu Jun 22, 2017 6:33 pm
by James_Ball
Are you doing SPME on the headspace or in the liquid sample?

In the liquid there would be a lot of other organics competing for the adsorption sites on the fiber.

The low d4 recovery could be indicating that you are getting low recovery of the native analyte also. The good thing is you know how much you are recovering and can correct for that.

I have only seen loss of deuterium on labeled analytes when there is extreme pH values, such that when dropping pH to 1 or below you can get a peak that shows masses for multiple deuterium masses, such that a d10 analyte shows spectrum for a mixture of d10,d9,d8, ect all eluting near the same time.