Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 24: Determination of maleic acid and maleic anhydride in food simulants

This document, part of EN 13130, specifies an analytical procedure for the determination of maleic acid in the four conventional food simulants, water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil or approved substitute. The level of maleic acid determined is expressed as milligrams of maleic acid per kilogram of food or food simulant. The method is appropriate for the quantitative determination of maleic acid in approximate analyte concentration range of 5 mg/kg to 60 mg/kg in the above mentioned food simulants.
This method is also suitable for the determination of maleic anhydride in the four food simulants as the anhydride is hydrolyzed rapidly and completely to maleic acid during sample preparation. The level of maleic anhydride is then expressed as milligrams of maleic acid per kilogram of food simulant.
NOTE   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants, e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides. The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be found necessary to use sunflower oil or HB 307 if unacceptable interferences are found with olive oil.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 24: Bestimmung von Maleinsäure und Maleinanhydrid in Prüflebensmitteln

Diese Technische Spezifikation, Teil der EN 13130, legt ein Analyseverfahren zur Bestimmung von Maleinsäure in den vier üblichen Prüflebensmitteln Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung und Olivenöl oder ein zugelassenes Ersatzmittel fest. Der ermittelte Gehalt an Maleinsäure wird in Milligramm Maleinsäure je Kilogramm Lebensmittel oder Prüflebensmittel angegeben. Das Verfahren eignet sich zur quantitativen Bestimmung von Maleinsäure im angenäherten Konzentrationsbereich des Analyten von 5 mg/kg bis 60 mg/kg in den vorstehend angegebenen Prüflebensmitteln.
Dieses Verfahren ist auch für die Bestimmung von Maleinanhydrid in den vier Prüflebensmitteln geeignet, weil das Anhydrid während der Probenvorbereitung schnell und vollständig zu Maleinsäure hydrolysiert. Der Gehalt an Maleinanhydrid wird dann in Milligramm Maleinsäure je Kilogramm Prüflebensmittel angegeben.
ANMERKUNG   Das Verfahren sollte auch auf andere wässrige Prüflebensmittel sowie weitere fettige Prüflebensmittel, z. B. Sonnenblumenöl, Maiskeimöl oder eine Mischung synthetischer Triglyceride, anwendbar sein. Die Eignung der Fettsimulanz Prüflebensmittels sollte vor Beginn der Migrationsprüfungen beurteilt werden - es kann sich als erforderlich herausstellen, Sonnenblumenöl oder HB 307 zu verwenden, wenn bei der Verwendung von Olivenöl unannehmbare Störwirkungen auftreten.

Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matières plastiques soumises à des limitations - Partie 24 : Détermination de l'acide maléique et de l'anhydre maléique dans les simulants d'aliments

Le présent document qui fait partie de l'EN 13130, spécifie un mode opératoire d'analyse pour la détermination de l'acide maléique dans les quatre simulants d'aliments suivants : eau, solution aqueuse d'acide acétique à 3 % (m/v), solution aqueuse d'éthanol à 15 % (v/v) et huile d'olive ou produit de substitution approuvé. La teneur en acide maléique déterminée est exprimée en milligrammes d'acide maléique par kilogramme de simulant d'aliments. Cette méthode convient pour la détermination quantitative de l'acide maléique, pour une gamme de concentrations d'analyte comprise approximativement entre 5 mg/kg et 60 mg/kg dans l'un des simulants d'aliments mentionnés ci-avant.
Cette méthode convient également pour la détermination quantitative de l'anhydre maléique dans les quatre simulants d'aliments car l'anhydre maléique est hydrolysé rapidement et complètement en acide maléique pendant la préparation de l'échantillon. La teneur en anhydre maléique est exprimée en milligrammes d'acide maléique par kilogramme de simulant d'aliments.
NOTE   Il convient que la méthode puisse également être appliquée à d'autres simulants aqueux ainsi qu'à d'autres simulants gras, tels que l'huile de tournesol, l'huile de maïs ou un mélange de triglycérides synthétiques. Il convient d'évaluer l'aptitude à l'emploi du simulant gras avant de conduire les essais de migration ; l'utilisation d'huile de tournesol ou de HB 307 peut s'avérer nécessaire en cas d'interférences inacceptables dans l'huile d'olive.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 24. del: Določevanje maleinske kisline in anhidrida maleinske kisline v modelnih raztopinah za živila

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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 13130-24:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHPDOHLQVNHNLVOLQHLQDQKLGULGD
PDOHLQVNHNLVOLQHYPRGHOQLKUD]WRSLQDK]DåLYLOD

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

- Part 24: Determination of maleic acid and maleic anhydride in food simulants

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

die Beschränkungen unterliegen - Teil 24: Bestimmung von Maleinsäure und
Maleinanhydrid in Prüflebensmitteln

Matériaux et objets en contact avec les denrées alimentaires - Substances dans les

matieres plastiques soumises a des limitations - Partie 24 : Détermination de l'acide

maléique et de l'anhydre maléique dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-24:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-24:2005 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 13130-24:2005
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 13130-24:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-24
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 24: Determination of
maleic acid and maleic anhydride in food simulants

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

alimentaires - Substances dans les matières plastiques - Substanzen in Kunststoffen, die Beschränkungen

soumises à des limitations - Partie 24 : Détermination de unterliegen - Teil 24: Bestimmung von Maleinsäure und

l'acide maléique et de l'anhydre maléique dans les Maleinanhydrid in Prüflebensmitteln

simulants d'aliments

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 13130-24:2005: E

worldwide for CEN national Members.
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SIST-TS CEN/TS 13130-24:2005
CEN/TS 13130-24:2005 (E)
Contents
page

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

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

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

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

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

4 Reagents ................................................................................................................................................ 6

5 Apparatus .............................................................................................................................................. 8

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

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

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

9 Confirmation........................................................................................................................................ 13

10 Test report ........................................................................................................................................... 15

Bibliography ..................................................................................................................................................... 16

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SIST-TS CEN/TS 13130-24:2005
CEN/TS 13130-24:2005 (E)
Foreword

This document (CEN/TS 13130-24:2005) 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
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SIST-TS CEN/TS 13130-24:2005
CEN/TS 13130-24:2005 (E)

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

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 13130-24:2005
CEN/TS 13130-24:2005 (E)
Introduction

Maleic acid, C H O , PM/Ref. No 19540, and maleic anhydride, C H O , PM/Ref. No 19960, are

4 4 4 4 2 3

monomers used in the manufacture of certain plastics materials and articles intended to come into

contact with foodstuffs. After manufacture residual maleic acid and maleic anhydride can remain in

the finished product and may migrate into foodstuffs coming into contact with that product.

This method describes the determination of the specific migration of maleic anhydride as maleic acid.

The method has been pre-validated by a collaborative trial with three laboratories.

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SIST-TS CEN/TS 13130-24:2005
CEN/TS 13130-24:2005 (E)
1 Scope

This document, part of EN 13130, specifies an analytical procedure for the determination of maleic

acid in the four conventional food simulants, water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous

ethanol and olive oil or approved substitute. The level of maleic acid determined is expressed as

milligrams of maleic acid per kilogram of food or food simulant. The method is appropriate for the

quantitative determination of maleic acid in approximate analyte concentration range of 5 mg/kg to 60

mg/kg in the above mentioned food simulants.

This method is also suitable for the determination of maleic anhydride in the four food simulants as

the anhydride is hydrolyzed rapidly and completely to maleic acid during sample preparation. The

level of maleic anhydride is then expressed as milligrams of maleic acid per kilogram of food simulant.

NOTE The method should also be applicable to other aqueous food simulants as well as to the other fatty

food simulants, e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides. The suitability of the fat simulant

should be assessed prior to setting up migration tests - it may be found necessary to use sunflower oil or HB 307

if unacceptable interferences are found with olive oil.
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 maleic acid is determined by reverse phase, ion pair high performance liquid

chromatography (HPLC) with UV detection at 220 nm. Maleic anhydride hydrolyzes rapidly and

completely to maleic acid during sample preparation. Quantification of maleic acid is achieved using

citraconic acid, as an internal standard, with calibration against relevant food simulants samples,

fortified with known amounts of maleic acid.

Confirmation of the maleic acid level is carried out by ion exchange chromatography with UV

detection at 245 nm.
4 Reagents

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

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SIST-TS CEN/TS 13130-24:2005
CEN/TS 13130-24:2005 (E)
4.1 Analytes
4.1.1 Maleic acid, HO CCH=CHCO H purity greater than 98 %.
2 2

4.1.2 Citraconic acid, HO CC(CH )=CHCO H of purity greater than 98 % w/w and not containing

2 3 2
maleic acid.

4.1.3 Mesaconic acid, HO CH=C(CH ).CO H of purity greater than 98 % w/w and not containing

2 3 2
maleic acid.
NOTE Mesaconic acid may be used as an alternative internal standard.
4.2 Chemicals
4.2.1 Ethanol, absolute.
4.2.2 Sodium hydrogen carbonate
4.2.3 Water, HPLC grade.
4.2.4 Dipotassium hydrogen orthophosphate, K HPO .3 H O.
2 4 2
4.2.5 Potassium dihydrogen orthophosphate, KH PO
2 4.
4.2.6 Orthophosphoric acid (85 %)
4.2.7 Sodium hydroxide, 2 mol/l solution in water.
4.2.8 Cetyl trimethyl ammonium bromide, HPLC grade.
4.2.9 Disodium tetraborate
4.2.10 Ammonium chloride
4.2.11 Acetonitrile
4.3 Solutions
4.3.1 Stock solution of maleic acid in ethanol (7 500 mg/l)

Weigh accurately approximately 0,75 g of the maleic acid (4.1.1) into a tared 100 ml volumetric flask.

Half fill the flask with ethanol (4.2.1), shake thoroughly and make the volume up to the mark with

ethanol (4.2.1).
Calculate the actual concentration of maleic acid in milligrams per litre.
Repeat the procedure to provide a second stock solution.

NOTE The stock solutions can be stored at – 20 °C for up to 2 months in stoppered glass volumetric flasks.

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SIST-TS CEN/TS 13130-24:2005
CEN/TS 13130-24:2005 (E)
4.3.2 Preparation of an internal standard solution of citraconic acid in ethanol
(7 500 mg/l)

Weigh approximately 0,75 g of citraconic acid (4.1.2) into a tared 100 ml volumetric flask. Dissolve in

ethanol (4.2.1) and make the volume up to the mark with the ethanol.
4.3.3 Preparation of standard solutions of maleic acid in ethanol

Into six 50 ml volumetric flasks, add by pipette 0 ml, 0,5 ml, 1,0 ml, 2,0 ml, 5,0 ml, and 10,0 ml of the

stock solution (4.3.1). Add by pipette 5,0 ml of the internal standard solution (4.3.2). Dilute to the mark

with ethanol (4.2.1) to give standard solutions containing nominal concentrations of 0 mg/l, 75 mg/l,

150 mg/l, 300 mg/l, 750 mg/l, and 1 500 mg/l of maleic acid. Calculate the exact concentrations of the

standard solutions in milligrams per litre.

Repeat the procedure using the second stock solution prepared in 4.3.1 to give a second set of

standard solutions.

NOTE The standard solutions of maleic acid can be stored for up to 3 months in the stoppered glass flasks

at any temperature between 5 °C and 20 °C.
4.3.4 Preparation of a 1,0 % w/v sodium hydrogen carbonate in water
Dissolve 10 g of sodium hydrogen carbonate (4.2.2) in 1 l of water (4.2.3).
4.3.5 Preparation of phosphate buffer solution, pH 7,0

Dissolve 114,12 g of dipotassium hydrogen orthophosphate (4.2.4) and 68,05 g of dihydrogen

potassium orthophosphate (4.2.5) in 400 ml of water (4.2.3), heating and stirring to dissolve. Allow to

cool and transfer to a 500 ml volumetric flask. Adjust the pH to pH (7,0 ± 0,1) as necessary with

concentrated orthophosphoric acid (4.2.6), or dilute sodium hydroxide (4.2.7). Make the volume up to

the mark with water (4.2.3).
4.3.6 Preparation of the high performance liquid chromatography mobile phase

Store the mobile phase for a maximum of five days in a stoppered flask at room temperature.

It is important that the following procedure is followed rigidly in order to ensure a consistent and

reproducible separation of the maleic acid from the internal standard.

Weigh 1,80 g of cetyl trimethyl ammonium bromide (4.2.8) into a 200 ml glass beaker. Dissolve in

100 ml of water (4.2.3), warming as necessary in a water bath, and transfer rinsing well with water to

a 1 l volumetric flask. Add 200 ml of the phosphate buffer (4.3.5), using a measuring cylinder. Fill the

flask to just below the neck with water (4.2.3), and shake thoroughly to mix. Adjust the pH to

pH (6,6 ± 0,05) by adding concentrated orthophosphoric acid (4.2.6). Make the volume up to the mark

with water (4.2.3). Transfer the solution to the high performance chromatograph solvent reservoir, add

250 ml of acetonitrile, mix thoroughly and de-gas by sonification.

NOTE It may be necessary to filter the solution before use in order to remove any solid parts. De-gassing

may also be carried out by means of a helium flow, however foaming of the solution may be a problem.

Therefore sonificati
...

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