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    De bepaling van N-nitrosodimethylamine (NDMA) in bier via extractie met vaste stof matrix dispersie en GC-TEA meting

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    Authors
    Koole A
    Vaessen HAMG
    Type
    Report
    Language
    nl
    
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    Title
    De bepaling van N-nitrosodimethylamine (NDMA) in bier via extractie met vaste stof matrix dispersie en GC-TEA meting
    Translated Title
    The determination of N-nitrosodimethyl-amine (NDMA) in beer by matrix dispersion solid phase extraction and GC-TEA detection
    Publiekssamenvatting
    Voor de bepaling van N-nitrosodimethylamine (NDMA) in bier is een methode onderzocht die is gebaseerd op extractie via vaste stof matrix dispersie aan Celite en GC-TEA meting. De hieruit voortgekomen werkwijze is beschreven in de bijlage en is voorzien van prestatiekenmerken verkregen uit onderzoek van 11 monsters bier die zo veel mogelijk verschilden in matrix. Alle monsters zijn tenminste in duplo onderzocht. Het NDMA-gehalte varieerde van gemiddeld 0,09 tot gemiddeld 0,26 mug/kg. Voor monster 93M0198 werd een gemiddeld NDMA-gehalte gemeten van 0,13 mug/kg (N=6) met een variatiecoefficient van 9,5 %. Voor de overige 10 monsters is de herhaalbaarheid, uitgedrukt als het procentuele verschil van de individuele meetresultaten t.o.v. het gemiddelde meetresultaat per monster, gelijk aan of beter dan 15%. In totaal zijn 15 opbrengstexperimenten uitgevoerd waarbij het niveau van verrijken met NDMA respectievelijk 0,2 ; 0,5 en 1,0 mug/kg bedroeg. De gemiddelde terugwinning bedroeg 100 +/- 6%. De grenzen van detectie en bepaalbaarheid zijn berekend op basis van 4 blanco-bepalingen met als resultaat dat de voorlopige detectiegrens wordt geschat op ca. 0,05 mug/kg en de grens van bepaalbaarheid op ca. 0,1 mug/kg. De NDMA-bepaling in bier via vaste stof matrix dispersie en GC-TEA meting is eenvoudig uit te voeren en is aanzienlijk sneller, maar minder gevoelig, dan de tot nu toe gebruikte combinatie van vacuumdistillatie en GC-TEA meting.
    The determination of N-nitrosodimethylamine (NDMA) is beer by matrix dispersion solid phase extraction on Celite and GC-TEA detection was studied. The procedure that came out is described in the Annex and was labeled with performance characteristics resulting from the analysis of 11 beer samples differing in matrix composition as widely as possible. All samples were assayed, at least, in duplicate. NDMA levels found ranged, on average from 0.09 to 0.26 mug/kg. Sample 93M0198 contained on average (N=6) 0.13 mug/kg of NDMA and the coefficient of variation was 9.5%. For the remaining samples the repeatability, calculated as the difference in procent of the individual result versus the average result of the sample, is 15% or better. In all, 15 recovery experiments were carried out at NDMA spiking levels of 0.2 - 0.5 and 1.0 mug/kg. On average the recovery was 100 +/- 6%. The limit of detection and of quantitation were calculated from the results of 4 blank determinations, resulting in a tentative value of about 0.05 mug/kg and of about 0.1 mug/kg respectively. The determination of NDMA in beer by matrix dispersion solid phase extraction and GC-TEA detection is easy to handle and much faster, but less sensitive, then the combination of vacuum distillation and GC-TEA detection used so far.
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    HIGB
    URI
    http://hdl.handle.net/10029/256542
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