SIST-TS CEN/TS 13130-14:2005
(Main)Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants
This document, part of EN 13130, specifies an analytical procedure for the determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil or approved substitute. The level of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone determined, is expressed as milligrams of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone per kilogram of food or food simulant. The method is applicable to the quantitative determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in an approximate analyte concentration range of 0,18 mg/kg to 4/ kg of food simulants.
NOTE 1 The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. a mixture of synthetic triglycerides or sunflower oil.
NOTE 2 The suitability of the fat simulant should be assessed prior to setting up migration tests. Olive oil has been found to give unacceptable interference in some cases.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 14: Bestimmung von 3,3-Bis(3-Methyl-4-Hydroxyphenyl)-2-Indolinon in Prüflebensmitteln
Dieses Dokument, Teil der EN 13130, legt ein Analyseverfahren zur Bestimmung von 3,3-Bis(3-Methyl-4-Hydroxyphenyl)-2-Indolinon in den Prüflebensmitteln Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung, Olivenöl oder einem zugelassenen Ersatzmittel fest. Der ermittelte Gehalt an 3,3-Bis(3-Methyl-4-Hydroxyphenyl)-2-Indolinon wird in Milligramm 3,3-Bis(3-Methyl-4-Hydroxyphenyl)-2-Indolinon je Kilogramm Lebensmittel oder Prüflebensmittel angegeben. Das Verfahren eignet sich zur quantitativen Bestimmung von 3,3-Bis(3-Methyl-4-Hydroxyphenyl)-2-Indolinon im angenäherten Konzentrationsbereich des Analyten von 0,18 mg/kg bis 4 mg/kg Prüflebensmittel.
ANMERKUNG 1 Das Verfahren sollte auch auf andere wässrige Prüflebensmittel sowie weitere fettige Prüflebensmittel, z. B. eine Mischung synthetischer Triglyceride oder Sonnenblumenöl, anwendbar sein.
ANMERKUNG 2 Die Eignung der Fettsimulanz sollte vor Beginn der Migrationsprüfungen beurteilt werden. Bei der Verwendung von Olivenöl traten in einigen Fällen unannehmbare Störwirkungen auf.
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 14 : Détermination de la 3,3-bis(3-méthyl-4-hydroxyphenyl)-2-indolinone 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 la 3,3-bis(3-méthyle-4-hydroxyphényl)-2-indolinone dans les quatre simulants d'aliments suivants : eau, solution aqueuse d'acide acétique a 3 % (m/v), solution aqueuse d'éthanol a 15 % (v/v) et huile d'olive ou produit de substitution approuvé. La teneur en 3,3-bis(3-méthyle-4-hydroxyphényl)-2-indolinone déterminée est exprimée en milligrammes de 3,3-bis(3-méthyle-4-hydroxyphényl)-2-indolinone par kilogramme de denrée alimentaire ou de simulant d'aliments. Cette méthode s'applique a la détermination quantitative de la 3,3-bis(3-méthyl-4-hydroxyphényl)-2-indolinone dans les échantillons d'essai, pour une gamme de concentrations d'analyte comprise entre 0,18 mg/kg et 4 mg/kg dans le simulant d'aliments.
NOTE 1 Il convient que la méthode puisse également etre appliquée a d'autres simulants aqueux ainsi qu'a des simulants gras tels que l'huile de tournesol ou un mélange de triglycérides synthétiques.
NOTE 2 ll convient d'évaluer l'aptitude a l'emploi du simulant gras avant de conduire les essais de migration. Des interférences inacceptables ont parfois été constatées avec l'huile d'olive.
Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 14. del: Določevanje 3,3-bis(3-metil-4-hidroksifenil)-2-indolinona v modelnih raztopinah za živila
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-14:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO 'RORþHYDQMHELV PHWLOKLGURNVLIHQLO
LQGROLQRQDYPRGHOQLKUD]WRSLQDK]DåLYLOD
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food
simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 14: Bestimmung von 3,3-Bis(3-Methyl-4-
Hydroxyphenyl)-2-Indolinon in Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 14 : Détermination de la 3,3-bis(3
-méthyl-4-hydroxyphenyl)-2-indolinone dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-14:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-14:2005 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 13130-14:2005
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SIST-TS CEN/TS 13130-14:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-14
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 14: Determination of 3,3-
bis(3-methyl-4-hydroxyphenyl)-2-indoline 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 14 : Détermination de la unterliegen - Teil 14: Bestimmung von 3,3-Bis(3-Methyl-4-
3,3-bis(3-méthyl-4-hydroxyphènyl)-2-indolinone dans les Hydroxyphenyl)-2-Indolinon 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 13130-14:2005: E
worldwide for CEN national Members.
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SIST-TS CEN/TS 13130-14:2005
CEN/TS 13130-14:2005 (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 . 10
8 Expression of results. 11
9 Confirmation. 13
10 Test Report . 14
Bibliography . 15
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SIST-TS CEN/TS 13130-14:2005
CEN/TS 13130-14:2005 (E)
Foreword
This document (CEN/TS 13130-14:2005) 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 13130-14:2005
CEN/TS 13130-14:2005 (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 13130-14:2005
CEN/TS 13130-14:2005 (E)
Introduction
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone, PM/Ref. 13600, C H NO , is a monomer used in
22 19 3
the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs.
After manufacture residual 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone can remain in the finished
product and may migrate into foodstuffs coming into contact with that product.
The method has been pre-validated by collaborative trial with two laboratories.
5
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SIST-TS CEN/TS 13130-14:2005
CEN/TS 13130-14:2005 (E)
1 Scope
This document, part of EN 13130, specifies an analytical procedure for the determination of 3,3-bis(3-
methyl-4-hydroxyphenyl)-2-indolinone in the food simulants water, 3 % w/v aqueous acetic acid, 15 %
v/v aqueous ethanol and olive oil or approved substitute. The level of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone determined, is expressed as milligrams of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone per kilogram of food or food simulant. The method is
applicable to the quantitative determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in an
approximate analyte concentration range of 0,18 mg/kg to 4/ kg of food simulants.
NOTE 1 The method should also be applicable to other aqueous food simulants as well as to the other fatty
food simulants e.g. a mixture of synthetic triglycerides or sunflower oil.
NOTE 2 The suitability of the fat simulant should be assessed prior to setting up migration tests. Olive oil has
been found to give unacceptable interference in some cases.
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 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in aqueous food simulants is determined
by reverse phase high performance liquid chromatography (HPLC) with UV detection at 235 nm. Fat
simulants are extracted with 80 % aqueous acetonitrile prior to HPLC analysis. Quantification is
achieved by calibration against samples of relevant food simulants, fortified with known amounts of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone. The level of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-
indolinone determined, is expressed as milligrams per kilogram of food simulant.
Confirmation of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone is carried out by reverse phase HPLC
using an analytical column of different polarity with UV detection at 280 nm.
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analyte
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone, (C H NO ) purity greater than 98 % w/w.
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CEN/TS 13130-14:2005 (E)
4.2 Chemicals
4.2.1 Ethanol, absolute
4.2.2 Acetonitrile, chromatography grade
4.2.3 Water, HPLC grade
4.2.4 Orthophosphoric acid, 80 %
4.3 Solutions
4.3.1 Stock solution of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in ethanol
(approximately 2 500 mg/l)
Weigh to the nearest 0,1 mg approximately 0,06 g of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone
(4.1) into a tared 25 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 exact concentration of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in milligrams per
litre.
Repeat the procedure to provide a second stock solution.
NOTE The stock solutions may be stored in the dark at room temperature for up to 3 months in stoppered
glass volumetric flasks.
4.3.2 Intermediate standard solutions of 3,3-bis(3-methyl-4 -hydroxyphenyl)-2-indolinone in
ethanol
Into six 25 ml volumetric flasks, add by pipette 0 ml, 0,1 ml, 0,5 ml, 1,0 ml, 2,0 ml and 4,0 ml of the
stock solution (4.3.1). Dilute to the mark with ethanol (4.2.1) to give standard solutions containing
nominal concentrations of approximately 0 mg/l, 10 mg/l, 50 mg/l, 100 mg/l, 200 mg/l and 400 mg per
litre of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone. 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
intermediate standard solutions.
Store the standard solutions of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone stored for up to
3 months in the stoppered glass flasks, protected from light, at room temperature.
4.3.3 Solvent A, HPLC mobile phase
Dissolve 0,7 ml of 80 % orthophosphoric acid (4.2.4) in 620 ml of water (4.2.3) and shake thoroughly
to mix. Add 380 ml of acetonitrile (4.2.2) to the mixture.
4.3.4 Acetonitrile in water, 80 %
Transfer using a measuring cylinder 100 ml of water (4.2.3) and 400 ml of acetonitrile (4.2.2) to a
500 ml screw cap bottle, shake to mix thoroughly.
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SIST-TS CEN/TS 13130-14:2005
CEN/TS 13130-14:2005 (E)
5 Apparatus
NOTE An instrument or item of apparatus is listed only where it is special, or made to a particular
specification, usual laboratory glassware and equipment being assumed to be available.
5.1 High performance liquid chromatograph, capable of pumping a binary mobile phase gradient,
equipped with an ultraviolet detector (UV) and fitted with an injection valve with a 10 µl injection loop.
5.2 High performance liquid chromatography analytical column, packed with a bonded,
reverse phase, fully end capped C18, 25 cm x 4,6 mm I.D, 5 µm particle size silica based packing
maintained at a constant temperature of 20 °C ± 1 °C. The analytical column should be allowed to
equilibrate at the correct flow rate for an hour. The analytical column shall be capable of resolving
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone from any interferences in the food simulant.
NOTE The retention of the 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone on the analytical column is
sensitive to the proportion of acetonitrile in the mobile phase. The mobile phase should be prepared with care
and an adjustment of ± 5 % v/v of acetonitrile is usually sufficient to obtain a suitable retention time.
For guidance, details of a column and chromatographic conditions, which have been found suitable, are given
below:
Column Spherisorb ODS 2, C18, 25 cm x 4,6 mm id, 5 µm
Mobile phase Reservoir A: Solvent A (4.3.3).
Reservoir B: 100 % acetonitrile
Gradient 100 % A held for 8 min; raised over 1 min to 100 %
...
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