CEN TS 13130-11-2005 Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 11 Determination of 11- aminoundecanoic acid in food simul.pdf

1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-11:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 11: Determination of 11-aminoundecanoic acid in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g

2、44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-11:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 580 460

3、57 6National forewordThis Draft for Development is the official English language version of CEN/TS 13130-11:2005.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 n

4、ot 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 of this Draft for Deve

5、lopment 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 taken on its status at t

6、he 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 the conversion into a

7、 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 document reference and clau

8、se 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 to in this document

9、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 of a contract. Users

10、 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 15 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since pub

11、licationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-11February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 11: Determination of 11-aminoundecanoic acid in

12、food simulantsMatriaux et objets en contact avec les denresalimentaires - Matires plastiques et substances soumises des limitations - Partie 11 : Dtermination de lacide 11-aminoundecanoque dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen,

13、 die Beschrnkungenunterliegen - Teil 11: Bestimmung von 11-Aminoundecansure in PrflebensmittelnThis 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 memb

14、ers 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 in the same way as for an EN and to make the CEN/TS availablepromptly at national level in

15、 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, Den

16、mark, 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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISC

17、HES 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 13130-11:2005: EDD CEN/TS 13130-11:20052 Contents page Foreword . 3 Introduction. 5 1 Scope 6 2 Nor

18、mative references 6 3 Principle . 6 4 Reagents 7 5 Apparatus. 9 6 Samples 9 7 Procedure. 11 8 Expression of results 12 9 Confirmation 14 10 Test report 14 Bibliography 15 DD CEN/TS 13130-11:20053 Foreword This document (CEN/TS 13130-11:2005) has been prepared by Technical Committee CEN/TC 194 “Utens

19、ils 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 con

20、tact 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 p

21、ublication 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

22、 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,

23、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 determin

24、ation 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

25、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

26、 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-a

27、minoundecanoic 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 4Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulantsPart 15: Deter

28、mination of 1,3-butadiene in food simulantsPart 16: Determination of caprolactam and caprolactam salt in food simulantsPart 17: Determination of carbonyl chloride in plasticsPart 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4-dihydroxybenzophenone and 4,4d

29、ihydroxybiphenyl in food simulantsPart 19: Determination of dimethylaminoethanol in food simulantsPart 20: Determination of epichlorohydrin in plasticsPart 21: Determination of ethylenediamine and hexamethylenediamine in food simulantsPart 22: Determination of ethylene oxide and propylene oxide in p

30、lasticsPart 23: Determination of formaldehyde and hexamethylenetetramine in food simulantsPart 24: Determination of maleic acid and maleic anhydride in food simulantsPart 25: Determination of 4-methyl-pentene in food simulantsPart 26: Determination of 1-octene and tetrahydrofuran in food simulantsPa

31、rt 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulantsPart 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

32、 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 S

33、pecification 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, C

34、zech 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. DD CEN/TS 13130-11:20055Introduction 11-aminoundecanoic

35、 acid, C11H23O2N, PM/Ref. No 12788 is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture, residual acrylamide can remain in the polymer and may migrate into foodstuffs coming into contact with that product. Th

36、is analytical method should be used in conjunction with EN 13130-1, which describes the procedures to be applied prior to the determination of 11-aminoundecanoic acid in food simulants. NOTE Although the method is applicable to olive oil, it should be taken into account that 11-aminoundecanoic acid

37、is unstable in olive oil during storage. Therefore the method should only be applied in case of short exposure periods with olive oil. Alternatively iso-octane could be used as a substitute fatty food simulant. DD CEN/TS 13130-11:200561 Scope This document, part of EN 13130, specifies a method for t

38、he determination of 11-aminoundecanoic acid in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol, olive oil and iso-octane. The level of 11-aminoundecanoic acid determined is expressed as milligrams per kilogram of food simulant. The method is appropriate for the quanti

39、tative determination of 11-amino-undecanoic acid in approximate analyte concentration range of 0,5 mg/kg to 10 mg/kg of food simulants. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited appli

40、es. 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 plast

41、ics 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 11-aminoundecanoic acid in food simulants is determined by preparing a derivative of 11-aminoundecanoic acid with a fluorescent compo

42、nent. The derivative is subsequently determined by high performance liquid chromatography (HPLC) and fluorescence detection. Quantification is achieved using the calibration curve method. NOTE A method for confirmation of the presence of 11-aminoundecanoic acid has not yet been established. DD CEN/T

43、S 13130-11:200574 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analyte 11-aminoundecanoic acid, C11H23O2N, molecular weight 201, purity greater than 99 %. NOTE The monomer is stable for a long period at room temperature if protected from light. 4

44、.2 Chemicals 4.2.1 Acetic acid, glacial 4.2.2 Acetic acid, 96 % 4.2.3 Acetone 4.2.4 di-Sodium tetraborate-10-hydrate, Na2B4O710. H2O4.2.5 Boric acid 4.2.6 Fluorescamine, 4-phenylspiro-furan 2-(3), 1-phthalan-3,3-dione 4.2.7 Iso-octane 4.2.8 Methanol 4.2.9 Nitrogen 4.2.10 Phosphoric acid 85 % 4.2.11

45、Sodium dihydrogen phosphate monohydrate 4.2.12 Sodium hydroxide 4.2.13 Water deionized (HPLC quality) 4.3 Solutions 4.3.1 Stock solution of 11-aminoundecanoic acid in water (1,25 mg/ml) Weigh to the nearest 0,1 mg approximately 60 mg of 11-aminoundecanoic acid in a 50 ml volumetric flask. Dissolve t

46、he 11-aminoundecanoic acid in the smallest possible volume, approximately 1 ml, of 96 % acetic acid (4.2.2) and fill the conical flask up to the mark with water (4.2.13). Calculate the actual concentration in milligrams 11-aminoundecanoic acid per millilitre of solution. Repeat the procedure to obta

47、in a second stock solution. DD CEN/TS 13130-11:20058The two primary standard solutions of analyte shall be checked against one another. The response factor, i.e. detector response divided by concentration of analyte solution, of the two primary standard solutions shall not differ more than 5 %. If t

48、here is agreement within 5 %, subsequent diluted standard solutions shall be made from only one of the primary standard solutions. If the levels of the two independently prepared stock solutions do not correspond to within 5 %, both stock solutions shall be discarded, and new solutions shall be prep

49、ared. 4.3.2 Stock solution of 11-aminoundecanoic acid in iso-octane (0,5 mg/ml) Weigh to the nearest 0,1 mg approximately 25 mg 11-aminoundecanoic acid in a 50 ml volumetric flask. Dissolve the 11-aminoundecanoic acid in approximately 5 ml 100% acetic acid (4.2.1) and fill up to the mark with iso-octane (4.2.7). Calculate the actual concentration of 11-aminoundecanoic acid in milligrams per millilitre solution. Repeat the procedure to obtain a second stock solution, see 4.3.1. 4.3.3 Diluted standard solution of 11-aminoundecanoic acid in aqueous foo