CEN/TS 13130-24:2005
(Main)Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 24: Determination of maleic acid and maleic anhydride in food simulants
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
General Information
- Status
- Published
- Publication Date
- 22-Feb-2005
- Technical Committee
- CEN/TC 194 - Utensils in contact with food
- Drafting Committee
- CEN/TC 194/SC 1/WG 2 - Methods of test for monomers
- Current Stage
- 6060 - Definitive text made available (DAV) - Publishing
- Start Date
- 23-Feb-2005
- Completion Date
- 23-Feb-2005
Overview
CEN/TS 13130-24:2005 specifies an analytical method for the determination of maleic acid and maleic anhydride migrating from plastics into conventional food simulants. Part of the EN 13130 series, this Technical Specification covers quantification in the four standard simulants - water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil (or approved fatty substitutes) - and expresses results as mg of maleic acid per kg of food or simulant. The method is appropriate for approximate analyte concentrations from 5 mg/kg to 60 mg/kg and was pre‑validated in a collaborative trial.
Key topics and requirements
- Analytes covered: maleic acid and maleic anhydride (the anhydride hydrolyses to maleic acid during sample preparation and is reported as maleic acid).
- Analytical principle: reverse‑phase ion‑pair high performance liquid chromatography (HPLC) with UV detection (main detection at 220 nm). Confirmation by ion‑exchange chromatography with UV detection (245 nm).
- Quantification strategy: use of an internal standard (citraconic acid; mesaconic acid may be an alternative) and calibration with fortified simulant standards.
- Sample matrix scope: validated for the four conventional simulants; the method notes applicability to other aqueous and fatty simulants (e.g., sunflower oil, corn oil, synthetic triglyceride mixes) but recommends verifying suitability of fat simulants before migration testing.
- Reagents and solutions: requirements for analytical‑grade reagents, preparation of stock and calibration solutions in ethanol, and a specific ion‑pair mobile phase formulation to resolve maleic acid from the internal standard.
- Performance and validation: method pre‑validated in an inter‑laboratory trial (three laboratories) and intended to support relevant EU plastics‑in‑contact‑with‑food directives.
Practical applications and users
Who benefits:
- Regulatory laboratories performing specific migration testing of plastics and food contact materials.
- Manufacturers of plastic food packaging and articles validating compliance with migration limits for maleic compounds.
- Quality control and R&D teams assessing residual monomers and their migration behavior into different food types (aqueous and fatty). Practical uses:
- Routine compliance testing against EU requirements for substances in plastics.
- Method development and confirmation when selecting alternative fatty simulants for migration studies.
- Generating quantitative migration data (mg/kg) for safety assessments and regulatory dossiers.
Related standards
- EN 13130-1: Guide to test methods and selection of conditions for food simulants (must be read in conjunction with this part).
- CEN/TS 13130 series: additional parts address determination of other monomers and additives in plastics (this part is one element of that series).
Keywords: CEN/TS 13130-24:2005, maleic acid, maleic anhydride, food simulants, plastics migration testing, ion‑pair HPLC, specific migration, food contact materials, EN 13130.
Frequently Asked Questions
CEN/TS 13130-24:2005 is a technical specification published by the European Committee for Standardization (CEN). Its full title is "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 standard covers: 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.
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.
CEN/TS 13130-24:2005 is classified under the following ICS (International Classification for Standards) categories: 67.250 - Materials and articles in contact with foodstuffs. The ICS classification helps identify the subject area and facilitates finding related standards.
You can purchase CEN/TS 13130-24:2005 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of CEN standards.
Standards Content (Sample)
SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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.
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
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
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.
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.
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.
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.
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
...
CEN/TS 13130-24:2005 문서는 식품과 접촉하는 물질 및 기사의 안전성을 보장하기 위한 중요한 표준으로, 특히 플라스틱 물질에 중점을 두고 있습니다. 이 표준의 범위는 남극산 및 남극무수물의 함량을 측정하는 분석 절차를 규명하며, 4가지 일반적인 식품 시뮬란트(물, 3% w/v 수용성 아세트산, 15% v/v 수용성 에탄올 및 올리브오일 또는 승인된 대체물)에서의 적합성을 포함하고 있습니다. 이 표준의 강점 중 하나는 남극산을 정량적으로 측정할 수 있는 정확한 방법을 제공한다는 것입니다. 분석은 5 mg/kg에서 60 mg/kg의 농도 범위에서 이루어지며, 측정된 남극산의 수준은 식품 또는 식품 시뮬란트의 킬로그램당 밀리그램으로 표현됩니다. 이러한 세밀한 접근은 식품 안전성을 확보하는 데 필수적입니다. 남극무수물의 측정 시 이 방법이 탁월한 이유는, 샘플 준비 과정에서 남극무수물이 즉시 남극산으로 하이드롤리시스 되므로, 동일한 분석 절차로 남극무수물의 함량을 평가할 수 있다는 점입니다. 이는 검출이 용이하다는 것을 의미하며, 표준이 다양한 식품 시뮬란트와의 호환성을 보장한다는 점에서 매우 유용합니다. 또한, 본 표준은 해바라기유, 옥수수유, 합성 트리글리세이드 혼합물과 같은 기타 지방성 식품 시뮬란트에 대해서도 적용 가능함을 명시하고 있습니다. 이를 통해 연구자는 다양한 시뮬란트에서 남극산 및 남극무수물 농도를 검토할 수 있는 유연성을 가지며, 특히 올리브오일에서의 간섭 문제가 발생할 경우 적합한 시뮬란트를 선택할 수 있는 지침을 제공합니다. 결론적으로, CEN/TS 13130-24:2005는 식품 접촉 물질의 안전성을 평가하기 위한 강력한 도구로, 남극산 및 남극무수물의 정량적 분석을 위한 신뢰할 수 있는 방법론을 제시하고 있습니다. 이 표준의 적용 가능성과 유용성은 식품 안전 연구에 있어 중요한 가치를 지니고 있으며, 앞으로의 연구 및 산업 적용에 필수적입니다.
The CEN/TS 13130-24:2005 standard is a critical document in the field of food safety, specifically focusing on materials and articles in contact with foodstuffs. The scope of this standard is to provide a detailed analytical procedure for the determination of maleic acid and maleic anhydride in various food simulants. This is particularly relevant as maleic acid and its anhydride form can pose risks to human health if present in food at certain levels. One of the key strengths of this standard is its thoroughness in specifying the four conventional food simulants: water, 3% w/v aqueous acetic acid, 15% v/v aqueous ethanol, and olive oil. By addressing these specific simulants, the standard allows for accurate and consistent measurement of maleic acid levels, expressed as milligrams per kilogram of food or food simulant. This quantitative approach is essential for regulatory compliance and ensuring safety in food products. Moreover, the standard not only targets maleic acid but also accommodates the determination of maleic anhydride, emphasizing the fact that it hydrolyzes rapidly to maleic acid during sample preparation. This dual capability enhances the relevance of CEN/TS 13130-24:2005, ensuring that both substances can be evaluated effectively in food safety assessments. In addition, the document hints at its adaptability, suggesting that the method may also be applicable to other aqueous and fatty food simulants, including sunflower oil and corn oil, which broadens the methodological applicability in practical scenarios. This flexibility is a significant advantage for laboratories and manufacturers who need to assess a variety of food contact materials. Overall, the CEN/TS 13130-24:2005 standard plays an essential role in food safety management, providing robust guidelines for the analysis of maleic acid and maleic anhydride. Its comprehensive scope, methodological rigor, and relevance to food safety regulations underscore its importance in ensuring that materials in contact with food are safe for consumer health.
Le document CEN/TS 13130-24:2005 apporte une contribution significative à la normalisation des matériaux et articles en contact avec les denrées alimentaires, notamment en ce qui concerne les substances plastiques soumises à limitation. Cette norme se concentre sur la détermination de l'acide maléique et de l'anhydride maléique dans les simulateurs alimentaires, une approche essentielle pour garantir la sécurité des produits alimentaires. L'étendue de cette norme est particulièrement pertinente, car elle établit une procédure analytique standardisée pour l'évaluation de la migration de l'acide maléique dans quatre simulateurs alimentaires conventionnels : l'eau, l'acide acétique aqueux à 3 % (m/v), l'éthanol aqueux à 15 % (v/v) et l'huile d'olive. Cela permet d'assurer une comparaison et une uniformité dans les tests de conformité entre différents matériaux en contact avec les aliments, renforçant ainsi la sécurité alimentaire. Parmi ses points forts, la norme offre une méthode quantitative précise pour déterminer l'acide maléique dans une plage de concentration analyte de 5 mg/kg à 60 mg/kg. En outre, elle permet également la détermination de l'anhydride maléique, qui se transforme rapidement en acide maléique lors de la préparation des échantillons, assurant ainsi une évaluation complète des risques associés à ces substances. La flexibilité de la méthode est un autre atout majeur. Bien qu'elle soit primordiale pour les quatre simulateurs mentionnés, le texte note également que cette méthode peut être adaptée à d'autres simulateurs alimentaires aqueux ainsi qu'à des simulateurs alimentaires gras, tels que l'huile de tournesol ou d'autres mélanges de triglycérides synthétiques. Cette adaptabilité est essentielle, car elle permet aux professionnels de la sécurité alimentaire de s'assurer que les matériaux utilisés sont conformes, quel que soit le type de simulateur employé. En résumé, la norme CEN/TS 13130-24:2005 se révèle être un outil indispensable pour l'industrie alimentaire et les laboratoires d'analyses, garantissant une évaluation efficace et fiable des risques associés à la migration de l'acide maléique et de l'anhydride maléique. Sa portée, sa précision et sa flexibilité en font un standard de référence incontournable pour assurer la sécurité des matériaux en contact avec les aliments.
CEN/TS 13130-24:2005は、食品に接触する材料および製品に関連する重要な標準であり、特に食品シミュラント中のマレイン酸およびマレイン無水物の定量的分析手法を明確に定義しています。この文書は、EN 13130の一部として、さまざまな食品シミュラント（水、3% v/v 酢酸水溶液、15% v/v エタノール水溶液、オリーブオイルまたは承認された代替品）におけるマレイン酸の測定を目的としています。 この標準の強みは、その定量的な分析能力にあります。特に、マレイン酸の濃度範囲が5mg/kgから60mg/kgの場合において、正確かつ信頼性のある結果を提供する点は高く評価されます。また、マレイン無水物も同様に迅速に水分解されてマレイン酸に変換されるため、マレイン無水物の定量にも適していることが本標準の特徴です。 さらに、この標準は、他の水性食品シミュラントや脂質基の食品シミュラント（ひまわりオイル、コーンオイル、合成トリグリセリドの混合物など）にも適用可能であると示唆されている点が重要です。これにより、幅広い食品シミュラントに対して汎用性が高まり、その結果、食品業界におけるマレイン酸およびマレイン無水物の管理が強化されるでしょう。 CEN/TS 13130-24:2005は、食品の安全性を確保するための重要な基準であり、食品処理業界における品質管理や規制遵守を実現するための重要なツールであるため、その関連性は非常に高いと言えます。このように、本標準は食品業界における装置およびプロセスの標準化を進め、安全性を高めるために不可欠な要素といえるでしょう。
Die Norm CEN/TS 13130-24:2005 behandelt Materialien und Artikel, die mit Lebensmitteln in Kontakt kommen, und konzentriert sich auf die Bestimmung von Maleinsäure und Maleinsäureanhydrid in Lebensmittelsimulanten. Sie stellt ein wichtiges Dokument dar, das eine analytische Vorgehensweise für die Bestimmung von Maleinsäure in vier herkömmlichen Lebensmittelsimulanten, darunter Wasser, 3 % w/v Essigsäure, 15 % v/v Ethanollösung und Olivenöl, festlegt. Der festgestellte Gehalt an Maleinsäure wird in Milligramm pro Kilogramm Lebensmittel oder Lebensmittelsimulant ausgedrückt. Ein bedeutender Vorteil dieser Norm ist die quantitative Bestimmung von Maleinsäure im Konzentrationsbereich von 5 mg/kg bis 60 mg/kg, was der praktischen Anforderung der Lebensmittelindustrie entspricht. Des Weiteren ist die Methode auch für die Bestimmung von Maleinsäureanhydrid geeignet, da das Anhydrid während der Probenvorbereitung schnell und vollständig zu Maleinsäure hydrolysiert wird. Dies erhöht die Relevanz dieser Norm, da sie die Sicherheit und Qualität von Lebensmitteln, die mit Plastiken in Kontakt kommen, gewährleistet. Ein weiterer bedeutender Aspekt ist die Flexibilität der Norm. Sie sollte auch für andere wässrige Lebensmittelsimulanten sowie fettige Lebensmittelsimulanten wie Sonnenblumenöl und Maisöl anwendbar sein. Dies erweitert das Anwendungsspektrum erheblich und ermöglicht eine breitere Anwendung in den unterschiedlichsten Tests zur Migration. Die Norm legt zudem fest, dass die Eignung des Fett-Simulanten vor der Durchführung von Migrationstests bewertet werden sollte, was eine praxisnahe Herangehensweise darstellt und sicherstellt, dass keine unerwünschten Wechselwirkungen bei der Verwendung von Olivenöl auftreten. Zusammenfassend lässt sich sagen, dass die CEN/TS 13130-24:2005 eine fundamentale Richtlinie für die Überwachung von Kunststoffen in Kontakt mit Lebensmitteln bietet und damit einen entscheidenden Beitrag zur Lebensmittelsicherheit sowie zur Einhaltung der geltenden Vorschriften leistet.
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