We try to develop a method for quantification of 25 allergens at a level of 10 ppm. The most important allergens are cinnamaldehydes, coumarin and lyral. We use a AT-WAX (60m*0.25mm*0.25µm) with GC-MS, splitless injection of perfumes 1:5 diluted. All the 25 allergens are good separated injecting a standard solution. When a sample is injected a lot of peaks are migrating between 70 and 90 minutes. In this time range the above mentioned allergens also migrate. Quantification is not possible. Who has any experience analyzing allergens in perfumes?

I would have thought that you shouldn't have any trouble using selected ion monitoring to quantify. At 70- 90 minutes are your peaks still sharp? A 30m column should do for this analysis.

Regards,

Ralph

My company uses HP-1 or HP-5 columns for perfume component analyses, use approx. 90 minute run at approx. 3 degrees/minute ramp. We built our own 3000 pattern GCMS library.

Durk,
If you are analysing the same list that I have, then you will have limonene and benzyl alcohol nearly co-eluting or co-eluting with a DB1 or DB5 type phase.
You may be able to quantitate on selected ions to distinguish between them. I have been considering using a Wax type phase but my samples contain components that need boiling off at high temperatures and most of my other analyses need a non-polar phase.
I use 30m x 0.25um x 0.25mm id.

Good Luck!

Thanks you all for your advice. Maybe I should try a shorter column (30 m). I saw an application of the Thermo group using deconvolution software. Does anyone has experience with AMDIS for example. Is this the solution for all the co-eluting peaks?

Durk

Durk,

I know that LECO corporation sell a GC-MS system called Pegasus which utilises fast GC and decovolution software. There is plenty of info at www.leco.com It seems very impressive.

You might try the new SGE SOLGEL-Wax column. I have used it for a different analysis and have heated the column up to 280C without seeing any adverse effects.

In regards to AMDIS, I have seen believable results, and others that I have my doubts about. My impression is that it can be a very useful tool, but the user has to carefully examine the results to make sure they make sense.

Durk,
Are you still out there??
Look at the European Flavour and Fragrance Association (EFFA) website and they have a suggested method.

David

Anonymous,

Yes, I'm still here. I searched the EFFA site for the method but can't find the method. Do you refer to the method of IFRA. If so I saw this one. I'm not satisfied about that method because they don't give quality parameters (LOD and LOQ). Also there is no information about real samples. I now use a SolgelWax column and I have till now satisfying results.

Durk

Have a look on shimadzu europe. They have developped a method with QP2010 and SPME.

Can someone suggest me a GCMS system for small size fragrance industry