SIST EN 16852:2017

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 alkoholischen Getränken - 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 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

• Status: Published
• Public Enquiry End Date: 29-Jul-2015
• Publication Date: 05-Jun-2017
• ICS: 67.160.10 - Alcoholic beverages
• Technical Committee: KŽP - Agricultural food products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 05-May-2017
• Due Date: 10-Jul-2017
• Completion Date: 06-Jun-2017
• Directive: 2014/34/EU - Directive 2014/34/EU Of The European Parliament And Of The Council of 26 February 2014 on the harmonisation of the laws of the Member States relating to equipment and protective systems intended for use in potentially explosive atmospheres (recast)
• Directive: 882/2004 - Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 onofficial controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules
• Mandate: M/463 - Mandate for Standardisation addressed to CEN for the methods of analysis for food contaminants
• Ref Project: EN 16852:2017 - Foodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and other spirit drinks - GC-MS method

Overview

EN 16852:2017 (CEN) defines a validated analytical method for the determination of ethyl carbamate (EC) in stone fruit spirits, fruit marc spirits and other spirit drinks using gas chromatography with mass spectrometric detection (GC‑MS). The standard covers two sample approaches: a simplified direct injection for low‑dry‑extract samples and a sample clean‑up using solid phase extraction (SPE) for sugared or high‑extract beverages. The method was validated by an interlaboratory study and demonstrates proven linearity across practical concentration ranges.

Key topics and technical requirements

• Scope & validation
  • Validated levels in interlaboratory study: 0.253 mg/l to 1.11 mg/l.
  • Proven linearity: 0.10–4.0 mg/l (simplified method) and 0.025–3.0 mg/l (with sample clean‑up).
• Analytical principle
  • GC‑MS in single ion monitoring (SIM) mode; examples use a PEG (DB‑WAX) capillary column.
  • Internal standards: butyl carbamate (BC) commonly used; deuterated d5‑ethyl carbamate also referenced.
• Sample preparation
  • Simplified method: direct injection for samples with total dry extract < 10 g/l after adjustment of alcoholic strength and addition of ISTD.
  • SPE clean‑up: diatomaceous earth based sorbent (e.g. Extrelut®), elution with cyclohexane/ethyl acetate, concentration of eluate (rotary evaporator conditions example: 25–30 kPa, 40 °C).
  • Use brown/light‑protected glassware to avoid light‑induced formation of EC from precursors.
• Quality & safety
  • Use analytical‑grade solvents and EN ISO 3696 water.
  • Ethyl carbamate is classified by IARC as probably carcinogenic - appropriate lab safety measures required.
• Reporting
  • Calibration by plotting EC/ISTD peak‑area ratios; report concentrations (mg/l) with two significant figures.

Applications and typical users

• Regulatory and official food control laboratories monitoring compliance in alcoholic beverages.
• Distilleries and beverage manufacturers conducting quality control and product safety testing for ethyl carbamate in stone fruit spirits, liqueurs and marc spirits.
• Contract analytical labs offering EC quantitation services using GC‑MS and SPE workflows.
• Research groups studying formation, mitigation and shelf‑life implications of EC in distilled products.

Related standards and references

• Normative reference: EN ISO 3696:1995 (water for analytical laboratory use).
• Prepared by CEN/TC 275 (Food analysis - Horizontal methods); national adoption required across CEN member states.

Keywords: EN 16852:2017, ethyl carbamate, EC, GC‑MS method, stone fruit spirits, fruit marc spirits, spirit drinks, SPE clean‑up, solid phase extraction, internal standard, analytical method, CEN.

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
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
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 workin
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