Anyone has experienced lose of recovery from volatile analytes that are traped by non volatile compunds in sample matrix?
I am using a method for fat soluble vitamins in oils but seens that my sample are traped in the injector,I am sure that I have vitamin but I can see nothing in some samples.
loong chain triglicerides are non volatile in 300ēC (my injector temperature)
any idea?
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By Anonymous on Wednesday, October 9, 2002 - 11:20 am:
Have you tried extacting the vitamins out of the sample matrix first?
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By Anonymous on Wednesday, October 9, 2002 - 11:46 am:
yes,but the triglycerides are very soluble in everything that the vitamin is:CHCl,Hexane,Acetone...
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By Anonymous on Wednesday, October 9, 2002 - 11:57 am:
Then you should try SPE to trap the triglycerides. I don't know what phase you would use but there may already be a method developed. Have you tried calling the chemistry/applications group at Waters (800-252-4752) or another chromatography company.
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By H W Mueller on Wednesday, October 9, 2002 - 11:32 pm:
We had this problem in the fatty acid analysis in plasma/serum. The coextracted lipids (TG, PL, ...) accumulated in the injector giving rise to slowly increasing discrimination (the higher FA started to decrease in concentration), J Chrom, 228, 75 (1982).
If your SPE, or whatever, doesn,t work 100% (how could it??) you can expect something of this sort. Many people do not see this, simply because they don´t do large enough series. Devising a cold injector which can be washed between each run (automatically) stopped this problem. It is hard to understand that the industry is not adopting this.
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By Anonymous on Thursday, October 10, 2002 - 08:28 am:
thanks everybody,
but what I think more strange is that some samples I have 2,3 or maybe 5% of vitamin and in the gas chromatogaph I see nothing,but in HPLC I see the peaks well,I already read about trap some analytes in injector but only when you have low concentrations,What I mean is :there is no doubt that my analytes are traped by noin volatile compunds ,there is?
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By Anonymous on Thursday, October 10, 2002 - 11:25 am:
If you can readily see the analytes of interest by LC why do you need to use GC?
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By Anonymous on Thursday, October 10, 2002 - 11:52 am:
in the GC I have a autosample and in the LC no.
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By Anonymous on Thursday, October 10, 2002 - 12:56 pm:
Is the method validated for GC? Sometimes you have to bite the bullet and spend money when you can't get a method to work. Have you looked into buying a demo or used autosampler for your LC? What kind of lab do you work in?
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By Anonymous on Thursday, October 10, 2002 - 01:45 pm:
other people in my lab(goverment lab for foods analysis)already quantitated Vitamins by GC but not in this matrix.
GC separations are more fast, I prefer put rotine analysis in a GC than in a LC.
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