prEN 16852

• Abstract:

  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.

• Status: Not Published
• Publication Date: 10-Apr-2028
• ICS: 67.160.10 - Alcoholic beverages
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 13 - Neoformed contaminants
• Current Stage: 4020 - Submission to enquiry - Enquiry
• Start Date: 15-Oct-2026
• Due Date: 22-Jul-2026
• Completion Date: 15-Oct-2026
• 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: oSIST prEN 16852:2026 - Foodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and other spirit drinks - GC-MS method

• Revises: EN 16852:2017 - Foodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and other spirit drinks - GC-MS method
• Effective Date: 09-Feb-2026

prEN 16852 is a draft European Standard from CEN for determining ethyl carbamate (EC) in stone fruit spirits, fruit marc spirits and other spirit drinks by gas chromatography with mass spectrometric detection. It is written for laboratories that need a GC-MS method for routine analysis, method validation, and comparison of EC results in these spirit matrices.

What does prEN 16852 specify?

prEN 16852 specifies a GC-MS method for measuring EC in stone fruit spirits, fruit marc spirits and other spirit drinks. The scope also notes that the method was validated in an interlaboratory study for stone fruit spirits and fruit liqueurs, and that the document separates a simplified direct-injection route from a clean-up route for more extract-rich samples.

The document is organized into:

• Clause 1 - scope
• Clause 4 - principle
• Clauses 5 to 6 - reagents and apparatus
• Clauses 7 to 11 - sample preparation, GC-MS conditions, calculation, precision and test report
• Annex A - typical chromatograms
• Annex B - precision data

Annex	What it covers
Annex A	Typical chromatograms for the simplified method and for the method with sample clean-up
Annex B	Precision data from the interlaboratory study

In practice, this structure helps a laboratory move from sample preparation to instrument setup, calibration, calculation, and reporting without having to assemble the method from several separate documents.

What are the key requirements of prEN 16852?

prEN 16852 gives two analytical routes, and the choice depends mainly on the dry extract in the sample. For samples with total dry extract below 10 g/l, the method uses direct GC-MS injection after adding an internal standard. For more extract-rich samples, the method uses solid phase extraction (SPE) clean-up first. This matters because concentrated extracts can reduce GC-MS sensitivity and make the measurement less reliable.

Sample handling and protection

prEN 16852 states that stone fruit spirits can form EC during storage when exposed to sunlight, so analysis should use light-protected glassware such as brown glass. In practice, this means the laboratory should avoid giving light a chance to change the EC content before the measurement is finished.

The method also allows the sample to be analysed either with or without adjustment of alcoholic strength for the simplified route. That gives laboratories a practical choice when matching standards and samples to the same alcohol level is important for the GC system being used.

Reagents, standards and quality control

prEN 16852 requires analytical-grade reagents, HPLC-quality solvents, and defined solutions for EC, butyl carbamate (BC) and deuterated ethyl carbamate (d-EC). It also adds a quality control (QC) sample requirement: an appropriate QC sample should be included in each sequence and treated like a routine sample. In practice, this gives the analyst a built-in check that the whole sequence is working as expected.

The standard also notes that other internal standards may be used in the simplified method if they give equivalent results. That gives laboratories some flexibility, but they still need to show that the alternative behaves like the specified internal standard.

GC-MS measurement

prEN 16852 uses gas chromatography with mass spectrometric detection in single ion monitoring (SIM) mode. The document gives example conditions for the column, injector, carrier gas and oven program, and it identifies the ions used for EC, BC and d-EC. It also allows other conditions if they can demonstrate similar performance. In practice, the laboratory can adapt the instrument setup, but it must still show that the method works comparably.

Calibration and calculation

prEN 16852 requires calibration standards to be injected at the start of each sequence, from the lowest to the highest concentration. The calibration is based on the peak area ratio of EC to the internal standard. If the sample response falls outside the calibrated range, the sample must be diluted and measured again. This is the core of the quantification step, so it is what links the chromatogram to the final result.

Precision and reporting

prEN 16852 summarizes repeatability and reproducibility from the interlaboratory study in Annex B, and it warns that those figures apply to the matrices and concentration ranges studied. The test report must identify the sample, cite the document, record the relevant dates, state the result with units, and mention any optional or nonstandard operations that could affect the result. That keeps results traceable and makes later review easier.

Who uses prEN 16852?

prEN 16852 is used by laboratories that analyse spirits for ethyl carbamate, especially laboratories working with stone fruit spirits, fruit marc spirits and fruit liqueurs. It is relevant to food analysis labs, beverage quality control teams, and official or contract laboratories that need a documented GC-MS procedure for EC testing.

It also matters to producers and quality managers in the spirits sector because EC is a contaminant that can be checked during product control, shelf-life studies and release testing. Buyers and specifiers may also use it when they need to name a specific analytical method for supplier or compliance checks.

What changed in prEN 16852 from the previous edition?

prEN 16852 will supersede EN 16852:2017. The document states these significant technical changes:

• removed normative references from the document
• added purity and CAS numbers for several reagents
• allowed different weights for standard substances or commercially available standard solutions
• added clause 5.22 on the QC sample
• removed the recommendation for a PTV injector
• added an optional sample preparation without adjusting alcoholic strength
• amended EC concentrations in the calibration solutions in Table 2
• added an optional qualifier ion
• added a calculation formula for the method with SPE clean-up
• removed the ISO 17025 reference from the test report requirements
• added alcoholic strength for matrices used in the method validation study
• full editorial revision

Which standards are used with prEN 16852?

The document cites EN ISO 1042 for one-mark volumetric flasks used in solution preparation. It also cites ISO 5725-2 in Annex B as the basis for the collaborative-study procedure behind the precision data.

What does the prEN 16852 document contain?

Clause 5 contains the reagent list, stock solutions and calibration solutions for both the simplified method and the clean-up method. Clause 7 gives the sample preparation routes, including the SPE clean-up sequence and the handling steps needed to protect samples from light.

Clause 8 gives example GC and MS conditions that laboratories can use as a starting point for method setup. Clause 9 explains the calibration graph and the calculation of EC concentration from the peak area ratios.

Annex A provides typical chromatograms for the two analytical routes, which helps analysts check peak shape and ion response during method verification. Annex B summarizes the precision data from the interlaboratory study, which is useful when assessing method performance for routine work or laboratory validation.

SLOVENSKI STANDARD
01-december-2026
Živila - Ugotavljanje etil karbamata v žganju iz koščičastega sadja, sadnih tropin in
v drugih žganih pijačah - Metoda GC-MS
Foodstuffs - Determination of ethyl carbamate in stone fruit spirits, fruit marc spirits and
other spirit drinks - GC-MS method
Lebensmittel - Bestimmung von Ethylcarbamat in Steinobstbränden, Bränden aus
Obsttrester und anderen Spirituosen - GC-MS-Verfahren
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
Ta slovenski standard je istoveten z: prEN 16852
ICS:
67.160.10 Alkoholne pijače Alcoholic beverages
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2026
ICS 67.160.10 Will supersede EN 16852:2017
English Version
Foodstuffs - Determination of ethyl carbamate in stone
fruit spirits, fruit marc spirits and other spirit drinks - GC-
MS method
Produits alimentaires - Détermination de la teneur en Lebensmittel - Bestimmung von Ethylcarbamat in
carbamate d'éthyle dans les eaux-de-vie de fruits à Steinobstbränden, Bränden aus Obsttrester und
noyaux, les eaux-de-vie de marc de fruits et les autres anderen Spirituosen - GC-MS-Verfahren
boissons alcoolisées - Méthode par CG-SM
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 275.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.

This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2026 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 16852:2026 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 7
7 Procedure . 8
7.1 General remarks . 8
7.2 Preparation of samples for simplified method, dry extract < 10 g/l . 8
7.2.1 Preparation of samples without adaption of alcoholic strength . 8
7.2.2 Preparation of samples using adaption of alcoholic strength . 8
7.3 Preparation of samples for method using sample clean-up . 9
8 Gas chromatography and mass spectrometry (GC-MS) . 9
8.1 GC conditions . 9
8.2 MS conditions . 9
9 Calculation . 10
10 Precision . 10
10.1 General . 10
10.2 Repeatability . 11
10.3 Reproducibility . 11
11 Test report . 11
Annex A (informative) Typical chromatograms . 13
A.1 Chromatograms of the simplified method . 13
A.2 Chromatograms of the method with sample clean up . 15
Annex B (informative) Precision data . 18
Bibliography . 19
European foreword
This document (prEN 16852:2026) has been prepared by Technical Committee CEN/TC 275 "Food
analysis - Horizontal methods", the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 16852:2017.
— Removed normative references from the document;
— added purity and CAS numbers for several substances in the reagents clause;
— included option to use different weights for standard substances or commercially available
standard solutions;
— added new clause 5.22 with information on quality control;
— removed recommendation about PTV injector for the GC device;
— included an optional sample preparation without the adjustment of the alcoholic strength;
— amended ethyl carbamate concentrations of the calibration solutions in Table 2;
— added an option for an additional qualifiér ion;
— added a calculation formula for the method with SPE clean-up;
— removed reference to ISO 17025 regarding test report requirements;
— added the alcoholic strength for matrices used in the method validation study;
— full editorial revision.
1 Scope
This European Standard spécifiés 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 (simplifiéd method) and 0,025 mg/l to 3,0 mg/l
(procedure including sample clean-up), respectively.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and définitions are listed in this document.
• ISO Online browsing platform: available at http://www.iso.org/obp
• IEC Electropedia: available at http://www.electropedia.org/
4 Principle
Samples 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 addition of internal standard (ISTD), and
optionally after the adjustment of the alcoholic strength of the beverage. Samples 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
influéncé 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.
5 Reagents
Use only reagents of recognized analytical grade, including deionized water, unless otherwise spécifiéd.
Solvents shall be of quality for HPLC (High Performance Liquid Chromatography) analysis.
In the preparation of solutions, other amounts can also be used respecting the given accuracy.
Commercially available solutions may also be used.
Ethyl carbamate has been classifiéd by IARC as probably carcinogenic to humans (see [1]).
5.1 Ethanol absolute, ≥ 99 %.
5.2 Ethanol solution, volume fraction φ = 65 %.
Pipet 65 ml of ethanol (5.1) into a 100 ml volumetric flask and fill to the mark with water.
5.3 Ethanol solution, φ = 35 %.
Pipet 35 ml of ethanol (5.1) into a 100 ml volumetric flask and fill to the mark with water.
5.4 Cyclohexane.
5.5 Ethyl acetate.
5.6 Eluant, cyclohexane + ethylacetate, V + V , 1+1.
1 2
5.7 n-Pentane.
5.8 Solid phase material.
Approximately 20 g of a chemically inert, wide-pore and highly pure diatomaceous earth based solid
® 1
phase, e.g. Extrelut NT
5.9 Sodium chloride.
5.10 Ethyl carbamate, ≥ 99 %, CAS 51-79-6.
5.11 Butyl carbamate, ≥ 98 %, CAS 592-35-8.
5.12 d -Ethyl carbamate, ≥ 98% chemical purity, ≥ 99% isotopic purity, CAS 73962-07-9.
5.13 Ethyl carbamate stock solution, mass concentration ρ(EC) = 1 000 mg/l.
Weigh to the nearest 0,01 mg, 50 mg of ethyl carbamate (5.10) into a 50 ml volumetric flask and fill to
the mark with ethanol (5.1).
5.14 Ethyl carbamate working solution 1, ρ(EC) = 100 mg/l.
Pipet 5 ml of ethyl carbamate stock solution (5.13) into a 50 ml volumetric flask and dilute to the mark
with ethanol (5.1).
5.15 Ethyl carbamate working solution 2, ρ(EC) = 10 mg/l.
Pipet 5 ml of ethyl carbamate working solution 1 (5.14) into a 50 ml volumetric flask and dilute to the
mark with ethanol (5.1).
5.16 Butyl carbamate stock solution, ρ(BC) = 1 000 mg/l.
Weigh to the nearest 0,01 mg, 50 mg of butyl carbamate (5.11) into a 50 ml volumetric flask and fill to
the mark with ethanol (5.1).
5.17 Butyl carbamate working solution, ρ(BC) = 40 mg/l.
Pipet 2 ml of butyl carbamate stock solution (5.16) into a 50 ml volumetric flask. Add 33 ml of ethanol
(5.1) and dilute to the mark with water.
5.18 d -Ethyl carbamate stock solution, ρ(d5-EC) = 1 000 mg/l.
Weigh to the nearest 0,01 mg, 50 mg of d -ethyl carbamate (5.12) into a 50 ml volumetric flask and fill
to the mark with ethanol (5.1).
5.19 d -Ethyl carbamate working solution, ρ(d5-EC) = 40 mg/l.
Pipet 2 ml of d -ethyl carbamate stock solution (5.18) into a 50 ml volumetric flask. Add 33 ml of ethanol
(5.1) and dilute to the mark with water.
5.20 Ethyl carbamate standard solutions for simplified method, dry extract < 10 g/l.
The ethyl carbamate standard solutions for the simplifiéd method can be prepared according to Table
1. A minimum of 6 standard solutions shall be prepared.
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.
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 (5.14 or 5.15) stated in Table 1 into a 10 ml volumetric flask and
add the corresponding amount of ethanol (5.1). Fill the volumetric flask to the mark with an ethanol
solution with a volume fraction of 65 % (5.2).
For an ethyl carbamate standard solution with a volume fraction of 40 %, use an ethanol solution with
a volume fraction of 35 % (5.3) to fill up the volumetric flasks.
Table 1 — Exemplary preparation of the ethyl carbamate standard solutions for simplified
method
Standard solution EC working solution EC working solution Ethanol (5.1) ρ(EC)
2 (5.15 ) 1 (5.14 )
μl μl μl 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 (5.17)
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 7.2) 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.
5.21 Ethyl carbamate standard solutions for method using sample clean up
The ethyl carbamate standard solutions for the method using sample clean up can be prepared
according to Table 2. A minimum of 6 standard solutions shall be prepared. Seal the GC vial with a septum
cap and mix the content thoroughly.
Table 2 — Exemplary preparation of ethyl carbamate standard solutions for method using
sample clean up
Standard EC working EC working d -EC Ethanol (5.1) ρ(EC) ρ(EC)
solution solution 2 solution 1
working
(in standard (in relation to
(5.15) (5.14)
solution
solution) 20 ml
(5.19)
sample)
μl μl μl μl mg/l mg/l
C0 0 - 100 900 0,00 0,00
C1 50 - 100 850 0,50 0,025
C2 200 - 100 700 2,00 0,10
C3 500 - 100 400 5,00 0,25
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