EN 16852:2017
(Main)Foodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and other spirit drinks - GC-MS method
Foodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and other spirit drinks - GC-MS method
This European Standard specifies a gas chromatographic method using mass spectrometric detection for the determination of ethyl carbamate (EC) in stone fruit spirits, fruit marc spirits and other spirit drinks.
The method has been validated in an interlaboratory study for stone fruit spirits and fruit liqueurs, at levels ranging from 0,253 mg/l to 1,11 mg/l. However, linearity of the instrument response was proven for the concentration ranges 0,10 mg/l to 4,0 mg/l (simplified method) and 0,025 mg/l to 3,0 mg/l (procedure including sample clean-up), respectively.
Lebensmittel - Bestimmung von Ethylcarbamat in Steinobstbränden, Obstbränden und anderen Spirituosen - GC-MS-Verfahren
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Ethylcarbamat (EC) in Steinobstbränden, Obst¬bränden und anderen Spirituosen mit Gaschromatographie und Massenspektrometrie (GC MS) fest.
Das Verfahren wurde in einem Ringversuch für Steinobstbrände und Obstliköre in Bereichen von 0,253 mg/l bis 1,11 mg/l validiert. Die Linearität des Ansprechverhaltens des Gerätes wurde jedoch für die Konzentrations¬bereiche von 0,10 mg/l bis 4,0 mg/l (vereinfachtes Verfahren) und von 0,025 mg/l bis 3,0 mg/l (Verfahren mit Probenreinigung) nachgewiesen.
Produits alimentaires - Détermination de la teneur en carbamate d'éthyle dans les eaux-de-vie de fruits à noyaux, les eaux-de-vie de marc de fruits et les autres boissons alcoolisées - Méthode par CG-SM
La présente Norme européenne spécifie une méthode de détermination de la teneur en carbamate d’éthyle (CE) par chromatographie en phase gazeuse couplée à une détection spectrométrique de masse dans les eaux-de-vie de fruits à noyaux, les eaux-de-vie de marc de fruits et les autres boissons spiritueuses.
La méthode a été validée lors d’un essai interlaboratoires sur les eaux-de-vie de fruits à noyaux et les liqueurs de fruits, à des niveaux compris entre 0,253 mg/l et 1,11 mg/l. Toutefois, la linéarité de la réponse de l’instrument a été prouvée pour la gamme de concentration de 0,10 mg/l à 4,0 mg/l (méthode simplifiée) et de 0,025 mg/l à 3,0 mg/l (mode opératoire comprenant la purification de l’échantillon), respectivement.
Živila - Ugotavljanje etil karbamata v žganju iz koščičastega sadja, sadnih tropin in drugih žganih pijačah - Metoda GC-MS
Ta evropski standard določa metodo plinske kromatografije z uporabo masne spektrometrične detekcije za ugotavljanje etil karbamata v žganju iz koščičastega sadja, sadnih tropin in drugih žganih pijačah.
Ta metoda je bila validirana v medlaboratorijski študiji o žganju iz koščičastega sadja in sadnih likerjih v obsegu 0,253–1,11 mg/l. Kljub temu je bil linearni odziv instrumenta dokazan za koncentracije 0,10–4,0 mg/l (poenostavljena metoda) in 0,025–3,0 mg/l (postopek, vključno s čiščenjem vzorcev).
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Ethylcarbamat in Steinobstbränden, Obstbränden und anderen alkoholischen Getränken - GC-MS-VerfahrenProduits alimentaires - Détermination de la teneur en carbamate d'éthyle dans les eaux-de-vie de fruits à noyaux, les eaux-de-vie de marc de fruits et les autres boissons alcoolisées - Méthode CG-SMFoodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and other spirit drinks - GC-MS method67.160.10Alcoholic beveragesICS:Ta slovenski standard je istoveten z:EN 16852:2017SIST EN 16852:2017en,fr,de01-julij-2017SIST EN 16852:2017SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16852
May
t r s y ICS
x yä s x rä s r English Version
Foodstuffs æ Determination of ethyl carbamate in stone fruit spiritsá fruit marc spirits and other spirit drinks æ GCæMS method Produits alimentaires æ Détermination de la teneur en carbamate d 5éthyle dans les eauxædeævie de fruits à noyauxá les eauxædeævie de marc de fruits et les autres boissons alcoolisées æ Méthode par CGæSM
Lebensmittel æ Bestimmung von Ethylcarbamat in Steinobstbrändená Obstbränden und anderen Spirituosen æ GCæMSæVerfahren This European Standard was approved by CEN on
t r February
t r s yä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
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t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x z w tã t r s y ESIST EN 16852:2017
Typical chromatograms . 12 Annex B (informative)
Precision data . 16 Bibliography . 17
=
65 %. Pipet 65 ml of ethanol (4.1) into a 100 ml volumetric flask and dilute to the mark with water. 4.2.2 Ethanol solution,
=
35 %. Pipet 35 ml of ethanol (4.1) into a 100 ml volumetric flask and dilute to the mark with water. 4.3 Cyclohexane. 4.4 Ethyl acetate. 4.5 Eluant, mixture of one part per volume of cyclohexane and one part per volume of ethyl acetate. SIST EN 16852:2017
> 99 %. 4.10 Butyl carbamate. 4.11 d5-Ethyl carbamate,
> 99 %. 4.12 Ethyl carbamate s = 1 000 mg/l. Weigh, to the nearest 0,01 mg, 50 mg of ethyl carbamate (4.9) into a 50 ml volumetric flask and dilute to the mark with ethanol (4.1). 4.13
= 100 mg/l. Pipet 5 ml of ethyl carbamate stock solution (4.12) into a 50 ml volumetric flask and dilute to the mark with ethanol (4.1). 4.14
= 10 mg/l. Pipet 5 ml of ethyl carbamate working solution 1 (4.13) into a 50 ml volumetric flask and dilute to the mark with ethanol (4.1). 4.15
= 1 000 mg/l. Weigh, to the nearest 0,01 mg, 50 mg of butyl carbamate (4.10) into a 50 ml volumetric flask and dilute to the mark with ethanol (4.1). 4.16 Butyl carb = 40 mg/l. Pipet 2 ml of butyl carbamate stock solution (4.15) into a 50 ml volumetric flask. Add 33 ml of ethanol (4.1) and dilute to the mark with water. 4.17 d5--EC) = 1 000 mg/l. Weigh, to the nearest 0,01 mg, 50 mg of d5-ethyl carbamate (4.11) into a 50 ml volumetric flask and dilute to the mark with ethanol (4.1).
1) This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products. Equivalent products may be used if they can be shown to lead to the same results. SIST EN 16852:2017
solution EC working
solution 2 (4.14) µl EC working
solution 1 (4.13) µl Ethanol (4.1) µl
ethyl carbamate mg/l C0 0 - 500 0,00 C1 100 - 400 0,10 C2 200 - 300 0,20 C3 500 - 0 0,50 C4 - 80 420 0,80 C5 - 100 400 1,00 C6 - 200 300 2,00 C7 - 300 200 3,00 C8 - 400 100 4,00 Fill the 10 ml volumetric flasks to the mark and add 0,25 ml of butyl carbamate working solution (4.16) into each of them with a pipette (to give a total volume of 10,25 ml). It is very important that the volumes of standard solutions and sample solutions (before an optional adjustment of the alcoholic strength, see 6.1) are equal. Usually, 10 ml are used. Mix the solution thoroughly and transfer an aliquot into a GC vial and seal the vial with a septum cap. 4.20 Ethyl carbamate standard solutions for method using sample clean up Pipet the amount of ethyl carbamate working solution as given in Table 2 into a GC vial and add the corresponding amount of ethanol (4.1) and 100 µl of d5-ethyl carbamate working solution (4.18). Seal the GC vial with a septum cap and mix the content thoroughly. SIST EN 16852:2017
ethyl carbamate mg/l for a sample of 20 ml C0 0 - 900 0,00 C1 50 - 850 0,025 C2 200 - 700 0,10 C3 500 - 400 0,25 C4 - 100 800 0,50 C5 - 150 750 0,75 C6 - 200 700 1,00 C7 - 400 500 2,00 C8 - 600 300 3,00 NOTE Data provided by the participants of the interlaboratory study has shown that it is possible to use different internal standards besides butylcarbamate (BC) as described above
for the simplified method (e.g. d5-ethyl carbamate, propyl carbamate (PC) or methyl carbamate (MC)). 5 Apparatus Usual laboratory equipment and, in particular, the following. One-mark volumetric flasks should comply with EN ISO 1042:1999 [2]. 5.1 Glass vials for GC analysis, brown glass with septum caps. 5.2 Columns for solid phase extraction (SPE), volume of 20 ml. 5.3 Rotary evaporator, with a water bath or a suitable concentration evaporator. 5.4 Gas chromatograph with mass spectrometric detector (GC-MS), capable of single ion monitoring (SIM), preferably equipped with a programmed temperature vaporizing (PTV) injector. PTV injection allows injecting larger extract volumes compared to split/splitless (SSL) injection. This provides larger signal intensities and could be advantageous with regards to the limit of detection (LOD). However, split/splitless injection was proven suitable for the scope of this European Standard during the method validation study by collabor
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