|
oSIST prEN 13130-13:2006
01-december-2006
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO 'RORþHYDQMHELV KLGURNVLIHQLO SURSDQD
%LVIHQROD$ YPRGHOQLKUD]WRSLQDK]DåLYLOD
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 13: Determination of 2,2bis(4-hydroxyphenyl)propane (Bisphenol A) in food
simulants
Werstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 13: Bestimmung von 2,2-Bis(4-Hydroxyphenyl)
Propan (Bisphenol A) in Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 13 : Détermination du 2,2-bis(4-
hydroxyphenyl)propane (Bisphénol A) dans les simulants d'aliments
Ta slovenski standard je istoveten z: prEN 13130-13
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
oSIST prEN 13130-13:2006 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
EUROPEAN STANDARD
DRAFT
prEN 13130-13
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2006
ICS 67.250 Will supersede CEN/TS 13130-13:2005
English Version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 13: Determination of
2,2bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants
Matériaux et objets en contact avec les denrées Werstoffe und Gegenstände in Kontakt mit Lebensmitteln -
alimentaires - Substances dans les matières plastiques Substanzen in Kunststoffen, die Beschränkungen
soumises à des limitations - Partie 13 : Détermination du unterliegen - Teil 13: Bestimmung von 2,2-Bis(4-
2,2bis(4-hydroxyphenyl)propane (Bisphenol A) dans les Hydroxyphenyl)Propan (Bisphenol A) in Prüflebensmitteln
simulants d'aliments
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee CEN/TC 194.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations which
stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other language
made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same
status as the official versions.
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, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 13130-13:2006: E
worldwide for CEN national Members.
---------------------- Page: 2 ----------------------
prEN 13130-13:2006 (E)
Contents Page
Foreword. 3
Introduction . 5
1 Scope. 5
2 Normative references. 5
3 Principle. 5
4 Reagents. 5
4.1 Analyte. 6
4.2 Chemicals. 6
4.3 Solutions. 6
5 Apparatus. 7
6 Samples. 7
6.1 Test sample preparation. 7
6.2 Blank sample preparation . 8
6.3 Calibration sample preparation . 8
7 Procedure. 9
7.1 HPLC analysis. 9
7.2 Calibration. 9
7.3 Execution of determination. 9
7.4 HPLC interferences. 9
8 Expression of results. 9
8.1 Calculation of analyte level. 9
8.2 Precision. 10
9 Test report. 11
Annex ZA (informative) Relationship of this European Standard with Regulation
1935/2004 and Commission Directive 2002/72/EC and associated Directives . 12
Bibliography . 13
2
---------------------- Page: 3 ----------------------
prEN 13130-13:2006 (E)
Foreword
This document (prEN 13130-13:2006) has been prepared by Technical Committee CEN/TC 194
“Utensils in contact with food”, the secretariat of which is held by BSI.This document was prepared by
Subcommittee SC 1 of TC 194 as one of a series of analytical test methods for plastics materials and
articles in contact with foodstuffs.
This document is currently submitted to the CEN Enquiry.
This document will supersede CEN/TS 13130-13:2005.
At the time of preparation and publication of this standard the European Union legislation relating to
plastics materials and articles intended to come into contact with foodstuffs is incomplete. Further
Regulations, 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.
EN 13130-13 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 with the determination of specific monomers and additives in plastics. The other Parts
of EN 13130 are as follows.
Part 1: Guide to the test methods for the specific migration of substances from plastics into
food 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 ethylene 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 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
3
---------------------- Page: 4 ----------------------
prEN 13130-13:2006 (E)
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-1-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
4
---------------------- Page: 5 ----------------------
prEN 13130-13:2006 (E)
Introduction
2,2-Bis(4-hydroxyphenyl)propane, herein referred to as Bisphenol A, C H O , PM/Ref. 13480, is a
15 16 2
monomer used in the manufacture of certain plastics materials and articles intended to come into
contact with foodstuffs. After manufacture residual Bisphenol A can remain in the finished product and
may migrate into foodstuffs coming into contact with that product.
1 Scope
This document, part of EN 13130, specifies a method for the determination of Bisphenol A in the food
simulants distilled water, 3 % w/v acetic acid aqueous, 10 % v/v ethanol aqueous solution and
rectified olive oil. The level of Bisphenol A monomer determined is expressed as milligrams
Bisphenol A per kilogram of food simulant. The method is applicable to the quantitative determination
of Bisphenol A at a minimum level of 0,002 mg/kg in aqueous food simulants and 0,009 mg/kg in olive
oil.
NOTE The method should also be applicable to other aqueous food simulants as well as to the other fatty
food simulants, sunflower oil and a mixture of synthetic triglycerides.
2 Normative references
This European Standard incorporates by dated and undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to and revisions of
any of these publications apply to this European Standard only when incorporated in it by amendment
or revision. For undated references the latest edition of the publication referred to applies, including
amendments.
EN 13130-1:2004, Materials and articles in contact with foodstuffs – Plastics substances subject to
limitation– Part 1: Guide to the test methods for the specific migration of substances from plastics into
food 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 Bisphenol A in aqueous food simulants is determined by high performance liquid
chromatography (HPLC) with fluorescence (FLD) detection. Olive oil test samples are extracted with a
mixture of water/methanol and the resultant solution analysed by HPLC. Calibration is achieved by
analysis of relevant simulants containing known amounts of Bisphenol A.
4 Reagents
NOTE All reagents should be of recognised analytical quality unless otherwise stated
5
---------------------- Page: 6 ----------------------
prEN 13130-13:2006 (E)
4.1 Analyte
2,2-bis(4-hydroxyphenyl)propane (Bisphenol A or 4,4'-(methylethylidene)-bisphenol or 4,4'-
isopropylidenediphenol), C H O , molecular weight: 228,28, purity >99 %
15 16 2
4.2 Chemicals
4.2.1 n-Hexane
4.2.2 Methanol
4.2.3 Water, deionised
4.3 Solutions
4.3.1 Extraction solvent, methanol/water = 85:100
Measure 85 ml of methanol (4.2.2) and 100 ml of water (4.2.3) and mix.
4.3.2 Mobile phase for HPLC, methanol/water = 70:30
Measure 500 ml of methanol (4.2.2) and 215 ml of water (4.2.3) and mix.
4.3.3 Stock solution of Bisphenol A in methanol at a defined concentration of approximately
0,75 mg/ml
Weigh to the nearest 0,1 mg approximately 75 mg of Bisphenol A (4.1.1) into a 100 ml volumetric
flask. Dissolve the Bisphenol A in methanol and make up to the mark with methanol (3.2.2).
Calculate the concentration in micrograms of Bisphenol A per millilitre of solution.
Store the solution in a well closed container in the dark for a maximum period of 3 months at any
temperature between +20 °C and –20 °C.
Repeat the pr
...