SIST 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 range 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
Dieses Dokument legt ein Verfahren zur Bestimmung von Ethylcarbamat (EC) in Steinobstbränden, Obst¬bränden und anderen alkoholischen Getränken mit Gaschromatographie und Massenspektrometrie (GC-MS) fest.
Das Verfahren wurde in einem Ringversuch für Steinobstbrände und Obstliköre im Bereich von 0,253 mg/l bis 1,11 mg/l validiert. Die Linearität des Ansprechverhaltens des Gerätes wurde jedoch für den Konzentrations-bereich 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
Le présent document 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
SIST EN 16852:2017
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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CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
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
EN 16852:2017 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Reagents . 4 5 Apparatus . 7 6 Procedure. 8 7 Gas chromatography and mass spectrometry (GC-MS) . 9 8 Calculation . 9 9 Precision . 10 10 Test report . 11 Annex A (informative)
Typical chromatograms . 12 Annex B (informative)
Precision data . 16 Bibliography . 17
SIST EN 16852:2017
EN 16852:2017 (E) 3 European foreword This document (EN 16852:2017) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2017, and conflicting national standards shall be withdrawn at the latest by November 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. WARNING — The use of this standard can involve hazardous materials, operations and equipment. This document does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this standard to take appropriate measures for ensuring the safety and health of the personnel prior to application of the standard and to fulfil statutory requirements for this purpose. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16852:2017
EN 16852:2017 (E) 4 1 Scope 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. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) 3 Principle Stone fruit spirits with a content of total dry extract of less than 10 g/l are injected directly into the gas chromatography mass spectrometry (GC-MS) system after the adjustment of the alcoholic strength of the beverage when indicated and addition of internal standard (ISTD). Sugared brandies, liqueurs and other spirit drinks with a higher total dry extract are first transferred onto a solid phase extraction (SPE) cartridge and the ethyl carbamate is eluted with a mixture of cyclohexane and ethyl acetate. Stone fruit spirits can contain precursors of ethyl carbamate which get transformed into EC under the influence of sunlight, e.g. during the shelf life of a spirit. To obtain the actual content of EC in the sample, light-protected glass ware (e.g. brown glass) shall be used during the analysis. 4 Reagents Use only reagents of recognized analytical grade and water complying with grade 1 of EN ISO 3696:1995, unless otherwise specified. Solvents shall be of quality for HPLC (High Performance Liquid Chromatography) analysis. Ethyl carbamate has been classified by IARC as probably carcinogenic to humans (see [1]). 4.1 Ethanol absolute. 4.2 Ethanol solutions. 4.2.1 Ethanol solution, volume fraction
=
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
EN 16852:2017 (E) 5 4.6 n-Pentane. 4.7 Solid phase material. Approximately 20 g of a chemically inert, wide-pore and highly pure diatomaceous earth based solid phase, e.g. Extrelut® NT1) 4.8 Sodium chloride. 4.9 Ethyl carbamate,
> 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
EN 16852:2017 (E) 6 4.18 d5--EC) = 40 mg/l. Pipet 2 ml of d5-ethyl carbamate stock solution (4.17) into a 50 ml volumetric flask. Add 33 ml of ethanol (4.1) and dilute to the mark with water. 4.19 Ethyl carbamate standard solutions for simplified method, dry extract < 10 g/l The injection of samples with a dry extract exceeding 10 g/l can lead to a rapid loss of sensitivity of the GC-MS system, depending on the type of liner and GC column used. For samples with higher dry extract content a sample clean up is recommended (see 6.2). Prepare the ethyl carbamate standard solutions for the simplified method according to Table 1. In principle it is possible to prepare the ethyl carbamate standard solutions to an alcoholic strength with a volume fraction of 40 % or 70 % depending on the GC system. For example, for an ethyl carbamate standard solution with a volume fraction of 70 %, pipet the amount of ethyl carbamate working solution (4.13 or 4.14) stated in Table 1 into a 10 ml volumetric flask and add the corresponding amount of ethanol (4.1). Fill the volumetric flask to the mark with an ethanol solution with a volume fraction of 65 % (4.2.1). For an ethyl carbamate standard solution with a volume fraction of 40 %, use an ethanol solution with a volume fraction of 35 % (4.2.2) to fill up the volumetric flasks. Table 1 — Preparation of the ethyl carbamate standard solutions for simplified method Standard
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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