SIST EN 12868:2017

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Artikel für Säuglinge und Kleinkinder - Verfahren zur Bestimmung der Abgabe von N-Nitrosaminen und N-Nitrosierbaren Stoffen aus Flaschen- und Beruhigungssaugern aus Elastomeren oder GummiArticles de puériculture - Méthodes pour déterminer la libération de N-nitrosamines et de substances N-nitrosables par les tétines et les sucettes en élastomère ou en caoutchoucChild use and care articles - Methods for determining the release of N-Nitrosamines and N-Nitrosatable substances from elastomer or rubber teats and soothers97.190Otroška opremaEquipment for childrenICS:Ta slovenski standard je istoveten z:EN 12868:2017SIST EN 12868:2017en,fr,de01-julij-2017SIST EN 12868:2017SLOVENSKI
STANDARDSIST EN 12868:2002/AC:2003SIST EN 12868:20021DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12868
January
t r s y ICS
{ yä s { r Supersedes EN
s t z x zã s { { {English Version
Child use and care articles æ Method for determining the release of Nænitrosamines and Nænitrosatable substances from elastomer or rubber teats and soothers Articles de puériculture æ Méthode pour déterminer la libération de Nænitrosamines et de substances Nænitrosables par les tétines et les sucettes en élastomère ou en caoutchouc
Artikel für Säuglinge und Kleinkinder æ Verfahren zur Bestimmung der Abgabe von NæNitrosaminen und Nænitrosierbaren Stoffen aus Babysaugern aus Elastomeren und Gummi This European Standard was approved by CEN on
u r October
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
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t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s t z x zã t r s y ESIST EN 12868:2017

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 Deviations (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.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 table 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 conditions . 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 SIST EN 12868:2017

Justification of an N-nitrosamine 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 substances. 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 substances . 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 determinations 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
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 flexible 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 elastomer 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 SIST EN 12868:2017

Suitable columns are normally glass columns with a length of approximately 450 mm and an internal diameter of (18 ± 2) mm or of length of approximately 300 mm and an internal diameter of (26 ± 2) mm. Columns may be equipped with a stoppered outlet (e.g. polytetrafluoroethylene stopper) to help adjusting the eluent flow. NOTE 2
Alternatively to self-prepared columns, suitable pre-filled SPE columns for single use are commercially available. They can be used provided that they are free from N-nitrosamines and of sufficient capacity. 6.4 Sintered glass frits for columns (6.3). 6.5 Evaporator flask, glassware for concentration step (8.7) or any suitable automated evaporator capable to reduce the volume of Extract A or B (60 ml or above, see 8.6) to (0,9 ± 0,1) ml. 6.6 Water bath, capable of maintaining temperatures in the range 40 °C to 60 °C. 6.7 GC glass vials with septa free from N-nitrosamines. 6.8 UV lamp suitable for confirmation of N-nitrosamines according to 10.1 a). Illumination of the highest concentration of the calibration solutions in a UV transparent vial within a reasonable time (1– 3 h) shall degrade N-nitrosamines and significantly decrease the intensity of their peaks. NOTE Longwave (365 nm) UV lamps have been shown to significantly decrease the intensity of peaks from the highest concentrated calibration standard solution, but midrange and shortwave UV lamps are generally also suitable. 6.9
UV transparent glass vials to be used for confirmation of N-nitrosamines according to 10.1 a). 6.10 pH-meter with minimum (±0,2) pH-relative accuracy. 6.11 Chemiluminescence detector (Thermal Energy Analyser, TEA, see A.7). 6.12 Gas Chromatography (GC). The GC system shall separate the N-nitrosamines named in this standard, such that their peak areas can be compared with that due to the internal standard (see 7.4). It shall also separate N-nitroamines (3.8) from the named N-nitrosamines. Should other than the N-nitrosamines named in this standard (Table 2) be found, the GC system shall be adaptable for their separation and identification. N-nitrosamines which cannot be identified shall be confirmed according to 10.1 a) and be quantified and reported as given in 9.1. NOTE Annex B provides an example for gas chromatography settings suitable to obtain the required separations. SIST EN 12868:2017

For each calibration level e, concentrations of the internal standard and of the individual N-nitrosamines in the solution are recorded as Cint, e and Ci, e, see 8.9.1 7.4 N-nitrosamine used as internal standard N-nitrosodiisopropylamine (NDiPA, CAS 601-77-4) or a suitable alternative can be used as internal standard. The internal standard solution shall be free from other N-nitrosamines, and have a concentration of approximately 200 ng/ml in ethanol (5.6). 8 Procedure 8.1 General The samples shall be kept at room temperature in closed containers and protected from light. Sample preparation shall avoid any contamination (including rubber gloves). The determination of N-nitrosamines and N-nitrosatable substances releasing from teats according to this standard shall be at least in duplicate (see A.6), including the sample preparation steps. Separate samples A and B shall be prepared including separate pre-boiling. Also, they shall be migrated separately (see A.5). The method recovery shall be (95 ± 30) % for each tested N-nitrosamine (Table 2) and for the internal standard (7.4). It is recommended to re-check the method recovery for each tested N-nitrosamine at suitable intervals to document performance. Any deviation from the following procedure shall be validated against the method of this standard for the whole range of the N-nitrosamines and N-nitrosatable substances tested (A7). However testing in duplicate, 8.2 to 8.4, the calculation of results (9), confirmation of N-nitrosamines (10) and analytical tolerances (11) shall be strictly followed. Table 3 shows the procedures for both Sample A and B and for the Blank. SIST EN 12868:2017

Blank Test (8.8)
Sample A Sample B
8.3 Sample A for determining N-nitrosatable substances 8.4 Sample B for determining N-nitrosamines 8.3.1 Preparation and pre-boiling 8.4.1 Preparation and pre-boiling 8.3.2 Preparation of Migrate A 8.4.2 Preparation of Migrate B 8.3.2 Preparation of Migrate Blank 8.3.3 Nitrosation of Migrate A and preparation of Solution A 8.4.3 Preparation of Solution B 8.3.3 Nitrosation of Migrate Blank and preparation of Solution Blank
8.5 Preparation of extraction columns for Solution A 8.5 Preparation of extraction columns for Solution B 8.5 Preparation of extraction columns for Solution Blank 8.6.1 Extraction of N-nitrosamines from Solution A to obtain Extract A 8.6.2 Extraction of N-nitrosamines from Solution B to obtain Extract B 8.6.1 Extraction of N-nitrosamines from Solution Blank to obtain Extract Blank 8.7.1 Concentration of N-nitrosamines in Extract A to obtain Concentrate A 8.7.2 Concentration of N-nitrosamines in Extract B to obtain Concentrate B 8.7.1 Concentration of N-nitrosamines in Extract Blank to obtain Concentrate Blank 8.2 Sample Preparation Feeding teats shall be taken as they are from the packaging or detached from containers (usually baby bottles). Soother teats shall be taken as a whole, including the bead. Therefore they shall be removed from the soother without cutting the teat, which may require destruction of the plastic parts of the soother. Any tool used to remove the teat from the soother shall not contaminate the teat. Where the soother teat covers part of the shield, the teat including that part should also be removed without any damage as a whole. When cutting of the teat is unavoidable, it shall be stated in the test report. For whole elastomer soothers or soothers having different parts made of elastomers, the elastomer components shall be separated and tested as separate samples. NOTE Different parts in whole elastomer soothers are for example teat, mouth shield and ring. These parts may have been manufactured by different technology or with different composition. SIST EN 12868:2017

± 30) ml of boiling water (5.1) and boil for 10 min. Remove them from the water with tweezers or tongs and shake off excess water. Transfer immediately into a flask as given in 8.3.2. For ready to use products (see 3.9), the boiling step shall be omitted, which shall be noted in the test report. The above amount of sample represents the necessary minimum. To achieve the necessary limits of detection, larger sample amounts may be used up to a maximum of 10 g. Ratios of sample to migrating solution shall be maintained and the volume of any glassware including separation columns, and the volume of reagents shall be proportionally increased during 8.3 to 8.6. See A.4. 8.3.2 Preparation of Migrate A (for determining N-nitrosatable substances) See A.2 Use a conical flask of a size (approximately 30 ml) suitable to hold the pieces of Sample A. The sample shall remain completely immersed in the artificial saliva salt solution. Place the sample pieces from 8.3.1 into the flask and add, by pipette, the volume of 4 ml per gram of sample (G(S) x 4 ml / g) of the artificial saliva salt solution (5.5). For example, if G(S) = 5,7 g, the volume of artificial saliva salt solution shall be (22,8 ± 0,5) ml. Close with a ground glass stopper and gently shake to ensure the pieces are completely immersed in the solution, and place the closed flask at (40 ± 2) °C for (24 ± 0,5) h in the oven (6.2). NOTE Complete immersion can be aided by addition of glass beads to the flask. After that time, remove the flask from the oven and vigorously shake 5 times by hand (see A.5). Open the flask and with tweezers or tongs, one by one lift the pieces out of the migrate, shake off excess migrate into the flask and remove from the flask, leaving the migrate in the flask. This is Migrate A. Proceed immediately to 8.3.3. SIST EN 12868:2017
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