1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-10:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 10: Determination of acrylamide in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40
2、g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-10:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 580 46058 4National
3、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 because the method was not evaluated
4、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 of this Draft for Development are r
5、equested 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 taken on its status at the end of its
6、 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 the conversion into a European Sta
7、ndard, 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 document reference and clause number and
8、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 to in this document may be found i
9、n 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 of a contract. Users are responsib
10、le for its correct application.Summary of pagesThis document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 15 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. N
11、o. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-10February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 10: Determination ofacrylamide in food simulantsMatriaux et ob
12、jets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 10 : Dtermination delacrylamide dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 10
13、: Bestimmung von Acrylamid inPrflebensmittelnThis 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 theircommen
14、ts, 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 availablepromptly at national level in an appropriate form. It is permissible to keep co
15、nflicting 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, Hu
16、ngary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de St
17、assart, 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 13130-10:2005: E2 Contents page Foreword .3 Introduction.5 1 Scope6 2 Normative references6 3 Principle .6 4 Reagents 6 5 Apparatus.7 6 Samples8 7 Pr
18、ocedure.9 8 Expression of results11 9 Confirmation 13 10 Test report14 Bibliography15 DD CEN/TS 13130-10:20053 Foreword This document (CEN/TS 13130-10:2005) 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 1
19、3130 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 article
20、s 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 plasti
21、cs 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
22、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
23、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 fo
24、llows. 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: D
25、etermination 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 fo
26、od 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-benzenedimethanam
27、ine in food simulants Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants DD CEN/TS 13130-10:20054 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: Determi
28、nation 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 4,4dihydroxybiphenyl in food simulants Part 19: Determination
29、 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 he
30、xamethylenetetramine 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-tri
31、azine 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 Specific
32、ation 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 t
33、he 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, Franc
34、e, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-10:20055 Introduction Acrylamide, PM/Ref. No 10630, is a monomer used in the manufactu
35、re of certain plastics materials and articles intended to come into contact with foodstuffs. After the manufacture, residual acrylamide can remain in the polymer and may migrate into foodstuffs coming into contact with that product. The method has been pre-validated in a validation experiment only b
36、y one laboratory (developing laboratory). NOTE 1 The analytical method described in this part of EN 13130 is the result of a study for the determination of the migration of acrylamide from plastic materials into food simulants. In the course of the study several problems were encountered and solutio
37、ns for these problems were incorporated in the final method. The most suitable and straightforward method is described in this part of EN 13130. The method was successfully pre-validated by the developing laboratory, using the four official EU food simulants to establish the precision data at the re
38、striction criterion. Also migration tests were performed with samples containing acrylamide as monomer in contact with the four simulants for 10 d at 40 C. Recovery of acrylamide from fortified simulants at the restriction level was found satisfactory. On testing of the method by a second laboratory
39、 it appeared that the testing laboratory was not able to achieve the required detection limit of 0,01 mg/kg. Therefore determination of the reproducibility was not performed by the testing lab. In addition the testing laboratory experienced difficulties with the stability of the base line when opera
40、ting the HPLC UV detector at 202 nm. Based on the problems encountered by the testing laboratory the method description was modified to make critical points more clear. NOTE 2 The confirmation method as given in this method description could be followed by the testing laboratory for water and olive
41、oil, although again the detection limit could not be achieved. The lowest possible level was approximately 0,02 mg/kg. In the determination of acrylamide in 15 % v/v aqueous ethanol and 3 % w/v aqueous acetic acid, separation of the simulant and acrylamide was problematic. The testing laboratory con
42、cluded that the method was not suitable for the intended purpose. When however, the migration experiment is carried out in a more favourable ratio of contact area to simulant then the level of determination can be increased by -at most- a factor of five. In that case problems with detection limit an
43、d base line stability will be much less, and the method may appear to be suitable for the intended purpose. Within the scope of the Standards, Measurement and Testing project “Monomers” it was not possible to re-test the method and therefore the method described is considered to be a useful analytic
44、al method, with limited validation data. Further testing is required to demonstrate that the method can be applied with the required accuracy and limit of detection. DD CEN/TS 13130-10:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of acrylamid
45、e in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and fat simulant. The level of acrylamide monomer determined is expressed as milligrams of acrylamide/kg of food simulant. The method is appropriate for the quantitative determination of acrylamide in approximate an
46、alyte concentration range of 0,01mg/kg to 0,1 mg/kg of food simulants. The method should also be applicable to other fat simulants. NOTE 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 a mixture of synthet
47、ic triglycerides 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 reference
48、d 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 substa
49、nces in plastics and the selection of conditions of exposure to food simulants. 3 Principle The level of acrylamide in food simulants is determined by direct injection of aqueous food simulants for analysis by high performance liquid chromatography with an ion exclusion column and ultra violet, UV, detection. Fat simulants are extracted with water and the aqueous extracts than analyzed by high performance liquid chromatography (HPLC). Quantification is achieved using external standards. Confirmation of the identity of acrylamide is established by means
