CEN TS 13130-13-2005 Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 13 Determination of 2 2- bis(4-hydroxyphenyl)propane (Bisp.pdf

1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-13:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3

2、g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-13:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 Septem

3、ber 2005ISBN 0 580 46075 4National forewordThis Draft for Development is the official English language version of CEN/TS 13130-10:2005.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publications and is of a provisional nature be

4、cause the method was not evaluated using recognized ring trial procedures. As a consequence there are no reproducibility data for the method. It should be applied on this provisional basis, so that information and experience of its practical application may be obtained.Comments arising from the use

5、of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated 2 years after its publication by the European organization so that a decision can be ta

6、ken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards.According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support

7、 the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1 Migration from plastics, at British Standards House, 389 Chiswick High Road, London W4 4AL, giving the docume

8、nt reference and clause number and proposing, where possible, an appropriate revision of the text.A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred

9、 to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions

10、 of a contract. Users are responsible for its correct application.Summary of pagesThis document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 13 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendm

11、ents issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-13February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 13: Determination of 2,2-bi

12、s(4-hydroxyphenyl)propane (Bisphenol A) in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 13 : Dtermination du2,2-bis(4-hydroxyphnyl) propane (Bisphnol A) dans lessimulants dalimentsWerkstoffe und Gege

13、nstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 13: Bestimmung von 2,2-Bis(4-Hydroxyphenyl)Propan (Bisphenol A) in PrflebensmittelnThis Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.The period

14、 of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit theircomments, 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 i

15、n the same way as for an EN and to make the CEN/TS availablepromptly 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 m

16、embers 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 Un

17、ited Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. CEN/TS 13130-13:2

18、005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle . 6 4 Reagents 7 5 Apparatus 7 6 Samples . 8 7 Procedure 9 8 Expression of results 10 9 Confirmation 11 10 Test report . 12 Bibliography . 13 DD CEN/TS 13130-13:20053 Foreword This document (CEN/TS 1313

19、0-13:2005) 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” an

20、d 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

21、 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 ar

22、e 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 shoul

23、d 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 p

24、lastics 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 s

25、ubstances 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 ch

26、loride 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: Determi

27、nation 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 DD CEN/TS 13130-13:20054 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants Part 14:

28、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

29、-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4-dihydroxybenzophenone and 4,4dihydroxybiphenyl in food simulants Part 19: Determination of dimethylaminoethanol in food simulants Part 20: Determination of epichlorohydrin in plastics Part 21: Determination of ethylenediamine and hex

30、amethylenediamine 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-me

31、thyl-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 ar

32、e 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 Techni

33、cal 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

34、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, Slove

35、nia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-13:20055 Introduction 2,2-bis(4-hydroxyphenyl)propane, hereinafter referred to as Bisphenol A, C15H16O2, PM/Ref. 13480, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact wi

36、th foodstuffs. After manufacture residual Bisphenol A can remain in the finished product and may migrate into foodstuffs coming into contact with that product. The method has been pre-validated by a collaborative trial with three laboratories. DD CEN/TS 13130-13:20056 1 Scope This document, part of

37、EN 13130, specifies a method for the determination of Bisphenol A in the food simulants water, 3 % w/v acetic acid aqueous, 15 % 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

38、 method is applicable to the quantitative determination of Bisphenol A at a minimum level of 0,2 mg/kg to 0,7 mg per kilogram of food simulants. 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 synt

39、hetic triglycerides. 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 13

40、130-1:2004, 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

41、exposure to food simulants. 3 Principle The level of Bisphenol A in aqueous food simulants is determined by high performance liquid chromatography (HPLC) with ultra violet (UV) detection. Olive oil test samples are extracted with a mixture of water/methanol and the resultant solution analyzed by HPL

42、C. Calibration is achieved by analysis of relevant simulants containing known amounts of Bisphenol A. Confirmation of Bisphenol A is carried out by diode array detection. DD CEN/TS 13130-13:20057 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Ana

43、lyte 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A or 4,4-(methylethylidene)-bisphenol or 4,4-isopropylidenediphenol), C15H16O2, molecular weight: 228,28, purity 99 %. 4.2 Chemicals 4.2.1 n-Hexane 4.2.2 Methanol 4.2.3 Water, deionized 4.3 Solutions 4.3.1 Extraction solvent, methanol/water = 1:1 Measu

44、re 100 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 0,38 mg/ml Weigh

45、to the nearest 0,1 mg approximately 37,5 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 (4.2.2). Calculate the concentration in micrograms of Bisphenol A per millilitre of solution. Repeat the procedure to obtain a

46、 second stock solution. NOTE The solution can be stored in a well closed container in dark for a maximum of 3 months at any temperature between +20 C and 20 C. 5 Apparatus NOTE An instrument or item of apparatus is listed only where it is special or made to a particular specification, usual laborato

47、ry glassware and equipment being assumed to be available. 5.1 High performance liquid chromatograph, preferably, equipped with an automatic 20 l loop injector and a variable wavelength UV detector connected to an integrator. 5.2 HPLC column, capable of separating Bisphenol A fully from peaks origina

48、ting from the simulants and/or solvents used. Appropriate operating conditions shall be established for the specific equipment used for the determination. DD CEN/TS 13130-13:20058 NOTE The following column has been found to be suitable: column: stainless steel 250 x 4,6 mm packed with C18 coated sph

49、erical silica gel, particle size 5 m, (load of 9 % carbon and end-capped); mobile phase: methanol/water 70 : 30 (4.3.2); flow rate: 1 ml/min; detection: UV 280 nm. 5.3 Mechanical shaker (Vortex) 5.4 Micro syringes, 10 l, 50 l and 1 000 l. 5.5 Test tubes, volume 10 ml, size 10 cm x 1,5 cm. 6 Samples 6.1 Test sample preparation 6.1.1 General Laboratory samples of the food simulants to be analyzed shall be obtained as described in EN 13130-1. Samples shall be kept refrigerated at + 4 C in closed containers with the exclusion of light. Analyte-fr