Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 11: Determination of 11-aminoundecanoic acid in food simulants

This document, part of EN 13130, specifies a method for the determination of
11-aminoundecanoic acid in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol, olive oil and iso-octane. The level of 11-aminoundecanoic acid determined is expressed as milligrams per kilogram of food simulant.
The method is appropriate for the quantitative determination of 11-amino-undecanoic acid in approximate analyte concentration range of 0,5 mg/kg to 10 mg/kg of food simulants.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 11: Bestimmung von 11-Aminoundecansäure in Prüflebensmitteln

Diese Technische Spezifikation, Teil der EN 13130, legt ein Verfahren zur Bestimmung von 11 Aminoundecansäure in den Prüflebensmitteln Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung, Olivenöl und Isooctan fest. Der ermittelte Gehalt an 11 Aminoundecansäure wird in Milligramm je Kilogramm Prüflebensmittel angegeben.
Das Verfahren eignet sich zur quantitativen Bestimmung von 11 Aminoundecansäure im angenäherten Konzentrationsbereich des Analyten von 0,5 mg/kg bis 10 mg/kg Prüflebensmittel.

Matériaux et objets en contact avec les denrées alimentaires - Matières plastiques et substances soumises à des limitations - Partie 11 : Détermination de l'acide 11-aminoundecanoïque dans les simulants d'aliments

Le présent document, qui fait partie de l'EN 13130, spécifie une méthode pour la détermination de l'acide 11-aminoundécanoïque dans les cinq simulants d'aliments suivants : eau, solution aqueuse d'acide acétique à 3 % (m/v), solution aqueuse d'éthanol à 15 % (v/v), huile d'olive et iso-octane. La teneur en acide 11-aminoundécanoïque déterminée est exprimée en milligrammes par kilogramme de simulant d'aliment.
Cette méthode convient pour la détermination quantitative de l'acide 11-aminoundécanoïque dans une gamme de concentrations d'analyte comprise approximativement entre 0,5 mg/kg et 10 mg/kg de simulants d'aliments.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 11. del: Določevanje 11-aminoundekanojske kisline v modelnih raztopinah za živila

General Information

Status
Published
Publication Date
22-Feb-2005
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
23-Feb-2005
Completion Date
23-Feb-2005

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SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-11:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHDPLQRXQGHNDQRMVNHNLVOLQHY
PRGHOQLKUD]WRSLQDK]DåLYLOD

Materials and articles in contact with foodstuffs - Plastics substances subject to limitation

- Part 11: Determination of 11-aminoundecanoic acid in food simulants

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,

die Beschränkungen unterliegen - Teil 11: Bestimmung von 11-Aminoundecansäure in
Prüflebensmitteln

Matériaux et objets en contact avec les denrées alimentaires - Matieres plastiques et

substances soumises a des limitations - Partie 11 : Détermination de l'acide 11-
aminoundecanoique dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-11:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-11:2005 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 13130-11:2005
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 13130-11:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-11
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 11: Determination of 11-
aminoundecanoic acid in food simulants

Matériaux et objets en contact avec les denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln

alimentaires - Matières plastiques et substances soumises - Substanzen in Kunststoffen, die Beschränkungen

à des limitations - Partie 11 : Détermination de l'acide 11- unterliegen - Teil 11: Bestimmung von 11-

aminoundecanoïque dans les simulants d'aliments Aminoundecansäure in Prüflebensmitteln

This Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their

comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available

promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)

until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,

Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,

Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 13130-11:2005: E

worldwide for CEN national Members.
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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)
Contents
page

Foreword .............................................................................................................................................................3

Introduction.........................................................................................................................................................5

1 Scope......................................................................................................................................................6

2 Normative references............................................................................................................................6

3 Principle .................................................................................................................................................6

4 Reagents ................................................................................................................................................7

5 Apparatus...............................................................................................................................................9

6 Samples..................................................................................................................................................9

7 Procedure.............................................................................................................................................11

8 Expression of results..........................................................................................................................12

9 Confirmation ........................................................................................................................................14

10 Test report............................................................................................................................................14

Bibliography......................................................................................................................................................15

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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)
Foreword

This document (CEN/TS 13130-11:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils

in contact with food”, the secretariat of which is held by BSI.

This part of EN 13130 has been prepared within the Standards, Measurement and Testing project, MAT1-

CT92-0006, “Development of Methods of Analysis for Monomers” and has been prepared by Subcommittee

(SC 1) of TC 194 "Utensils in contact with food" as one of a series of test methods for plastics materials and

articles in contact with foodstuffs.

This standard is intended to support Directives 2002/72/EC [1], 89/109/EEC [2], 82/711/EEC [3] and its

amendments 93/8/EEC [4] and 97/48/EC [5], and 85/572/EEC [6].

At the time of preparation and publication of this part of EN 13130 the European Union legislation relating to

plastics materials and articles intended to come into contact with foodstuffs is incomplete. Further Directives

and amendments to existing Directives are expected which could change the legislative requirements which

this standard supports. It is therefore strongly recommended that users of this standard refer to the latest

relevant published Directive(s) before commencement of a test or tests described in this standard.

This part of EN 13130 should be read in conjunction with EN 13130-1.

Further parts of EN 13130, under the general title Materials and articles in contact with foodstuffs - Plastics

substances subject to limitation, have been prepared, and others are in preparation, concerned with the

determination of specific migration from plastics materials into foodstuffs and food simulants and the

determination of specific monomers and additives in plastics. The parts of EN 13130 are as follows.

Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food

simulants and the determination of substances in plastics and the selection of conditions of exposure to food

simulants
Part 2: Determination of terephthalic acid in food simulants
Part 3: Determination of acrylonitrile in food and food simulants
Part 4: Determination of 1,3-butadiene in plastics
Part 5: Determination of vinylidene chloride in food simulants
Part 6: Determination of vinylidene chloride in plastics

Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants

Part 8: Determination of isocyanates in plastics
Part 9: Determination of acetic acid, vinyl ester in food simulants
Part 10: Determination of acrylamide in food simulants
Part 11: Determination of 11-aminoundecanoic acid in food simulants
Part 12: Determination of 1,3-benzenedimethanamine in food simulants

Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants

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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)

Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants

Part 15: Determination of 1,3-butadiene in food simulants
Part 16: Determination of caprolactam and caprolactam salt in food simulants
Part 17: Determination of carbonyl chloride in plastics
Part 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene,

1,4-dihydroxybenzene, 4,4’-dihydroxybenzophenone and 4,4’dihydroxybiphenyl in food simulants

Part 19: Determination of dimethylaminoethanol in food simulants
Part 20: Determination of epichlorohydrin in plastics

Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulants

Part 22: Determination of ethylene oxide and propylene oxide in plastics

Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants

Part 24: Determination of maleic acid and maleic anhydride in food simulants
Part 25: Determination of 4-methyl-pentene in food simulants
Part 26: Determination of 1-octene and tetrahydrofuran in food simulants
Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants
Part 28: Determination of 1,1,1-trimethylolpropane in food simulants
Parts 1 to 8 are European Standards. Parts 9 to 28 are Technical Specifications.

WARNING All chemicals are hazardous to health to a greater or lesser extent. It is beyond the

scope of this Technical Specification to give instructions for the safe handling of all chemicals, that

meet, in full, the legal obligations in all countries in which this Technical Specification may be

followed. Therefore, specific warnings are not given and users of this Technical Specification should

ensure that they meet all the necessary safety requirements in their own country.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following

countries are bound to announce this CEN Technical Specification: Austria, Belgium, Cyprus, Czech Republic,

Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland

and United Kingdom.
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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)
Introduction

11-aminoundecanoic acid, C H O N, PM/Ref. No 12788 is a monomer used in the manufacture of certain

11 23 2

plastics materials and articles intended to come into contact with foodstuffs. After manufacture, residual

acrylamide can remain in the polymer and may migrate into foodstuffs coming into contact with that product.

This analytical method should be used in conjunction with EN 13130-1, which describes the procedures to be

applied prior to the determination of 11-aminoundecanoic acid in food simulants.

NOTE Although the method is applicable to olive oil, it should be taken into account that 11-aminoundecanoic acid is

unstable in olive oil during storage. Therefore the method should only be applied in case of short exposure periods with

olive oil. Alternatively iso-octane could be used as a substitute fatty food simulant.

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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)
1 Scope
This document, part of EN 13130, specifies a method for the determination of

11-aminoundecanoic acid in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous

ethanol, olive oil and iso-octane. The level of 11-aminoundecanoic acid determined is expressed as milligrams

per kilogram of food simulant.

The method is appropriate for the quantitative determination of 11-amino-undecanoic acid in approximate

analyte concentration range of 0,5 mg/kg to 10 mg/kg of food simulants.
2 Normative references

The following referenced documents are indispensable for the application of this document. For dated

references, only the edition cited applies. For undated references, the latest edition of the referenced

document (including any amendments) applies.

EN 13130-1:2004, Materials and articles in contact with foodstuffs – Plastics substances subject to limitation –

Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food

simulants and the determination of substances in plastics and the selection of conditions of exposure to food

simulants.
3 Principle

The level of 11-aminoundecanoic acid in food simulants is determined by preparing a derivative of

11-aminoundecanoic acid with a fluorescent component. The derivative is subsequently determined by high

performance liquid chromatography (HPLC) and fluorescence detection. Quantification is achieved using the

calibration curve method.

NOTE A method for confirmation of the presence of 11-aminoundecanoic acid has not yet been established.

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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)
4 Reagents

NOTE All reagents should be of recognized analytical quality unless otherwise stated.

4.1 Analyte

11-aminoundecanoic acid, C H O N, molecular weight 201, purity greater than 99 %.

11 23 2

NOTE The monomer is stable for a long period at room temperature if protected from light.

4.2 Chemicals
4.2.1 Acetic acid, glacial
4.2.2 Acetic acid, 96 %
4.2.3 Acetone
4.2.4 di-Sodium tetraborate-10-hydrate, Na B O 10. H O
2 4 7 2
4.2.5 Boric acid
4.2.6 Fluorescamine, 4-phenylspiro-[furan 2-(3), 1-phthalan]-3,3-dione
4.2.7 Iso-octane
4.2.8 Methanol
4.2.9 Nitrogen
4.2.10 Phosphoric acid 85 %
4.2.11 Sodium dihydrogen phosphate monohydrate
4.2.12 Sodium hydroxide
4.2.13 Water deionized (HPLC quality)
4.3 Solutions
4.3.1 Stock solution of 11-aminoundecanoic acid in water (1,25 mg/ml)

Weigh to the nearest 0,1 mg approximately 60 mg of 11-aminoundecanoic acid in a 50 ml volumetric flask.

Dissolve the 11-aminoundecanoic acid in the smallest possible volume, approximately 1 ml, of 96 % acetic

acid (4.2.2) and fill the conical flask up to the mark with water (4.2.13).

Calculate the actual concentration in milligrams 11-aminoundecanoic acid per millilitre of solution.

Repeat the procedure to obtain a second stock solution.
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SIST-TS CEN/TS 13130-11:2005
CEN/TS 13130-11:2005 (E)

The two primary standard solutions of analyte shall be checked against one another. The response factor, i.e.

detector response divided by concentration of analyte solution, of the two primary standard solutions shall not

differ more than 5 %. If there is agreement within 5 %, subsequent diluted standard solutions shall be made

from only one of the primary standard solutions.

If the levels of the two independently prepared stock solutions do not correspond to within ± 5 %, both stock

solutions shall be discarded, and new solutions shall be prepared.
4.3.2 Stock solution of 11-aminoundecanoic acid in iso-octane (0,5 mg/ml)

Weigh to the nearest 0,1 mg approximately 25 mg 11-aminoundecanoic acid in a 50 ml volumetric flask.

Dissolve the 11-aminoundecanoic acid in approximately 5 ml 100% acetic acid (4.2.1) and fill up to the mark

with iso-octane (4.2.7).

Calculate the actual concentration of 11-aminoundecanoic acid in milligrams per millilitre solution.

Repeat the procedure to obtain a second stock solution, see 4.3.1.

4.3.3 Diluted standard solution of 11-aminoundecanoic acid in aqueous food simulants (25 µµg/ml)

Pipette 2 ml of the stock solution (4.3.1) into a series of three 100 ml volumetric flasks. Make up to the mark

with the appropriate aqueous food simulant, water, 3 % w/v aqueous acetic acid and 15 % v/v aqueous

ethanol.

Calculate the actual concentration 11-aminoundecanoic acid in micrograms per millilitre of aqueous food

simulant.
4.3.4 Phosphoric acid, 8,5 %

Pipette 10 ml of the 85 % phosphoric acid (4.2.10) into a measuring flask of 100 ml and make up to the mark

with water (4.2.13).
4.3.5 Phosphate buffer, 5 mM, pH 3

Weigh 690 mg of sodium dihydrogen phosphate monohydrate (4.2.11) and dissolve in approximately 900 ml

water (4.2.13). Adjust to pH (3 ± 0,2) by adding small portions of 8,5 % phosphoric acid (4.3.4). Make up to 1

litre with water (4.2.13).
4.3.6 Mobile phase for HPLC

Prepare a mixture of 300 ml of 5 mM phosphate buffer, pH 3 (4.3.5) with 700 ml of methanol (4.2.8).

NOTE Degassing the mobile phase may be necessary with some HPLC equipment.
4.3.7 Borate buffer, 400 mM, pH 9

Weigh 15,3 g of di-sodium tetraborate (4.2.4) and dissolve in approximately 90 ml water (4.2.13). Adjust to

pH (9 ± 0,2) by adding small portions of 5 % boric acid. Make
...

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