EN 12868-2017 en Child use and care articles - Method for determining the release of N-nitrosamines and N-nitrosatable substances from elastomer or rubber teats and soothers《儿童使用和护.pdf

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1、BS EN 12868:2017Child use and care articles Method for determining therelease of N-nitrosamines andN-nitrosatable substances fromelastomer or rubber teats andsoothersBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN 12868:2017 BRITISH STANDARDNational forewordThi

2、s British Standard is the UK implementation of EN 12868:2017.It supersedes BS EN 12868:1999 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee CW/1/4, Feeding, drinking and mouthing.A list of organizations represented on this committee can be obtained on

3、request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 88240 1 ICS 97.190 Compliance with a Briti

4、sh Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS EN 12868:2017EUROPEAN STANDARD NORME EUROPE

5、NNE EUROPISCHE NORM EN 12868 January 2017 ICS 97.190 Supersedes EN 12868:1999English Version Child use and care articles - Method for determining the release of N-nitrosamines and N-nitrosatable substances from elastomer or rubber teats and soothers Articles de puriculture - Mthode pour dterminer la

6、 libration de N-nitrosamines et de substances N-nitrosables par les ttines et les sucettes en lastomre ou en caoutchouc Artikel fr Suglinge und Kleinkinder - Verfahren zur Bestimmung der Abgabe von N-Nitrosaminen und N-nitrosierbaren Stoffen aus Babysaugern aus Elastomeren und Gummi This European St

7、andard was approved by CEN on 30 October 2016. 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. Up-to-date lists and bibliographical references concerni

8、ng such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into i

9、ts own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germ

10、any, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KO

11、MITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12868:2017 EBS EN 12868:2017EN 12868:2017 (E) 2 Contents Page European foreword . 5 Introduction

12、 6 1 Scope 7 2 Normative references 7 3 Terms and definitions . 7 4 Principle . 8 5 Reagents . 8 Table 1 Salts and their masses for 1 l of artificial saliva salt solution 9 6 Apparatus . 9 7 Standard Solutions of N-nitrosamines 11 7.1 General . 11 7.2 N-nitrosamines identified in teats . 11 Table 2

13、Names, abbreviated names and CAS numbers of N-nitrosamines relevant for this standard, and the necessary limits of quantification 11 7.3 Calibration solutions (for detector response) . 12 7.4 N-nitrosamine used as internal standard . 12 8 Procedure 12 8.1 General . 12 8.2 Sample Preparation. 13 8.3

14、Sample A (for determination of N-nitrosatable substances) 14 8.3.1 Preparation and pre-boiling 14 8.3.2 Preparation of Migrate A (for determining N-nitrosatable substances) See A.2 14 8.3.3 Nitrosation of Migrate A (see A.3) and preparation of Solution A 15 8.4 Sample B (for determination of N-nitro

15、samines) . 15 8.4.1 Preparation and pre-boiling 15 8.4.2 Preparation of Migrate B (for determining N-nitrosamines). 15 8.4.3 Preparation of Solution B 15 8.5 Preparation of extraction columns for Solutions A and B . 15 8.6 Extraction of N-nitrosamines . 16 8.6.1 From Solution A 16 8.6.2 From Solutio

16、n B 16 8.7 Concentration of N-nitrosamines . 16 8.7.1 In Extract A . 16 8.7.2 In Extract B . 17 8.8 Blank Test . 17 8.9 Analysis 17 8.9.1 Calibration function 17 8.9.2 Determination of sample concentration . 18 9 Calculation of results 18 9.1 General . 18 9.2 Variability of results and calculation o

17、f means . 19 9.2.1 Requirements for variability . 19 9.2.2 Test for variability . 19 9.2.3 Calculation of means . 19 BS EN 12868:2017EN 12868:2017 (E) 3 9.3 Amount of total N-nitrosatable substances migrating from Sample A, analysed and expressed as N-nitrosamines from Concentrate A . 20 9.4 Amount

18、of total N-nitrosamines migrating from Sample B, analysed and expressed as N-nitrosamines from Concentrate B . 20 10 Confirmation of N-nitrosamines . 20 11 Analytical tolerances . 21 11.1 General . 21 11.2 Analytical tolerances (see Annex F) . 21 12 Compliance 21 13 Test report 21 Annex A (informati

19、ve) Rationales . 23 A.1 General . 23 A.2 Migration Conditions (see 8.3.2) . 23 A.3 Nitrosation conditions (see 8.3.3) 23 A.4 Weight of sample used (see 8.3.1) 23 A.5 Separate migrations (see 8.3.2 and 8.3.3) . 24 A.6 Duplicate tests (see 8.1) . 24 A.7 TEA and alternative detectors . 24 A.8 Deviation

20、s (see 9.2, 9.3 and 11) 25 A.9 Main differences between this standard and EN 71-12 3 . 25 Annex B (informative) Suitable gas chromatographic method . 26 Figure B.1 GC Chromatogram of a calibration solution recorded by TEA . 27 Annex C (normative) Example of results calculation and test report . 28 C

21、.1 General . 28 C.2 Example for variability testing and means calculation for analytical results 28 Table C.1 Example for variability testing and means calculation for Sample A 29 Table C.2 Example for variability testing and means calculation for Sample B 29 C.3 Results calculation and results tabl

22、e for test report . 30 Table C.3 Example of Final results and their representation 31 C.4 Other Information for test report . 31 Annex D (informative) Alternative Methods . 32 D.1 General . 32 D.2 Liquid Chromatography (LC) 32 Table D.1 Gradient profile for the given HPLC conditions 33 D.3 MS/MS con

23、ditions . 33 Table D.2 Suitable MRM Transitions for MS/MS conditions 34 D.4 Confirmation and quantification of detected N-nitrosamines . 34 Table D.3 Maximum permitted tolerances for relative ion intensities 34 BS EN 12868:2017EN 12868:2017 (E) 4 Annex E (informative) Justification of an N-nitrosami

24、ne specific adjustment for NDiNA 36 Annex F (informative) Summary of the 2015 validation trial . 38 F.1 Outline 38 Table F.1 Sample Descriptions for Validation Trial 38 F.2 Initial statistical analysis N-nitrosatable substances 38 Table F.2 Mean data and calculations for total N-nitrosatable substan

25、ces 38 F.3 Reproducibility Limit for N-nitrosatable substances 39 Table F.3 Overall means for total N-nitrosatable substances by method . 39 Table F.4 Reproducibility limits for total N-nitrosatable substances by method 39 Table F.5 Reproducibility limits (mg/kg) for individual N-nitrosatable substa

26、nces . 40 F.4 Consideration of the NDiNA Reproducibility limit . 40 F.5 Initial statistical analysis N-nitrosamines . 40 Table F.6 Mean data and calculations for total N-nitrosamines . 40 F.6 Variability between Determinations 41 Table F.7 Summary of average repeatability limits for duplicate determ

27、inations of N-nitrosatable substances and N-nitrosamines 41 F.7 Summary of Conclusions and implications for EN 12868 42 Table F.8 Methods used by laboratories (after removal of outliers) . 42 Bibliography . 44 BS EN 12868:2017EN 12868:2017 (E) 5 European foreword This document (EN 12868:2017) has be

28、en prepared by Technical Committee CEN/TC 252 “Child use and care articles”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2017, and conflicting n

29、ational standards shall be withdrawn at the latest by July 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 12868:19

30、99. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. Compared to EN 12868:1999, this document contains the following significant changes: The common practice to perform at least double determinations has been made a requ

31、irement, including the preparation of samples. Sample preparation has been defined and simplified, reducing this source of interlaboratory variation. The pre-boiling and migration steps have been separated for the determination of N-nitrosamines and of N-nitrosatable substances, allowing use of the

32、same vessels and avoiding the possible loss of migrated substances. Amounts of sample have been adjusted, increasing the sample mass for the determination of N-nitrosatable substances. Extraction of N-nitrosamines from the aqueous migrates has been restricted to one method, reducing interlaboratory

33、variability. A rinsing step has been introduced to avoid variability due to possible loss of analytes. The calculation of results has been revised including a repeatability requirement for multiple determinations and taking into account state of the art analytical procedures. The confirmation of N-n

34、itrosamines and application of analytical tolerances have been clarified including a N-nitrosamine specific adjustment as suggested by the validation trial. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this

35、European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, S

36、lovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 12868:2017EN 12868:2017 (E) 6 Introduction It has been shown that feeding teats and soothers made of elastomer or rubber may release N-nitrosamines and substances capable of being converted into N-nitrosamines (N-nit

37、rosatable substances). The Scientific Committee for Food of the European Union has given the opinion that N-nitrosamines and N-nitrosatable substances may endanger human health owing to their toxicity 5. Hence in 1993, the European Commission issued Directive 93/11/EEC 1 controlling rubber and elast

38、omeric teats and soothers releasing these substances. The Directive also provided basic rules for determining the release of these substances and criteria for the method of analysis to be adopted. The purpose of this European Standard is to provide a detailed analytical method for the identification

39、 and determination of N-nitrosamines and N-nitrosatable substances released from teats and soothers in order that compliance with the requirements of Directive 93/11/EEC may be tested. This method has been validated. The testing laboratories should take special care to observe occupational health an

40、d safety standards. Persons using this European Standard should be familiar with normal laboratory practice. This European Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health

41、 practices and to ensure compliance with any national regulatory conditions. BS EN 12868:2017EN 12868:2017 (E) 7 1 Scope This European Standard specifies the method for determining N-nitrosamines and N-nitrosatable substances released from elastomer or rubber teats in contact with artificial saliva

42、salt solution for testing compliance with Directive 93/11/EEC. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the

43、 latest edition of the referenced document (including any amendments) applies. EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025) 3 Terms and de

44、finitions For the purposes of this document, the following terms and definitions apply. 3.1 teat flexible elastomeric part designed to be placed in the mouth 3.2 soother article which includes a teat and which is intended to satisfy the non-nutritive sucking need of children Note 1 to entry: Soother

45、s are also known as pacifiers or babies dummies. 3.3 feeding teat any teat that permits a child to obtain food or drink 3.4 elastomer material which undergoes substantial, elastic (fully reversible) deformation when put under stress and consisting of three-dimensional networks of cross-linked flexib

46、le polymers Note 1 to entry: The cross-links are chemical bonds generated by curing in rubbers (like natural rubber or synthetic rubber including silicones) or physical, thermo-reversible fixation points in thermoplastic elastomers (TPE) or the combination of both (TPEV). 3.5 rubber types of elastom

47、er 3.6 N-nitrosamine substance characterised by the N-nitroso functional group, N-NO, usually formed by the reaction of an amine with a nitrosating agent, e.g. nitrite, at acidic pH BS EN 12868:2017EN 12868:2017 (E) 8 3.7 N-nitrosatable substance substance which when released into the artificial sal

48、iva salt solution (5.5) and submitted to the conditions of step 8.3.3 undergoes nitrosation to form a N-nitrosamine 3.8 N-nitroamine substance characterized by the N-nitro functional group bonded to an amine, N-NO2, also called N-nitramine 3.9 ready to use product product intended to be used without

49、 the need to clean before first use, but may be reusable 4 Principle N-nitrosamines and N-nitrosatable substances are migrated into a nitrite-containing artificial saliva salt solution under specified conditions. Two migrations are carried out: migration A for the determination of N-nitrosatable substances (determined as N-nitrosamines from migrate A after nitrosation) and migration B for the determination of N-nitrosamines (from migrate B). After extraction from the migrate and concentration, the concentrates are ex