Technical guidelines on testing the migration of primary aromatic ...

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LOD = blank + 3 ⋅ s R,s R is the internal reproducibility for samples with a level of 2 µg PAA/L.1.4.3 RecoveryRecoveries of the 20 PAA in distilled water or 3 % acetic acid (from spiking at theconcentrations of 2-25 µg/l) was 89-107 %28
2 PROTOCOL B BY LC-MSThis procedure describes a method for the quantitative determination or primaryaromatic amines (PAAs) in acidic aqueous food simulant 3% acetic acid, by liquidchromatography coupled to mass spectrometry (LC-MS/MS). The objective is thedetermination of PAAs in the specific migration tests of food contact materials. Thisprotocol has been validated by a single laboratory validation by NRL-ES (ReferenceSendon et al, 2010). The method has been validated for 8 PAAs, which aresummarized in the table below, along with their corresponding working range inμg/kg simulant.Amine CAS Range μg/kg simulantm-Phenylenediamine (m-PDA) 108-45-2 ≥2,52,6-Toluenediamine (2,6-TDA) 823-40-5 ≥2,52,4-Toluenediamine (2,4-TDA) 95-80-7 ≥2,51,5- Diaminenaphthalene (1,5-DAN) 2243-62-1 ≥2,5Aniline (ANL) 62-53-3 ≥2,54,4’-Diaminodiphenylether (4,4’-DPE) 101-80-4 ≥2,54,4’-Methylenedianiline (4,4’-MDA) 101-77-9 ≥2,53,3’- Dimethylbenzidine (3,3-DMB) 119-93-7 ≥2,52.1 PrincipleThe acidic food simulant obtained in the migration test is submitted to neutralizationwith ammonia before chromatography analysis. Individual PAAs are separated on amixed-mode reverse phase C18 column and mass detection is performed usingpositive electrospray ionisation (ESI+), in multireaction monitoring mode (MRM).29
Page 1 and 2: Technical
Page 3 and 4: Executive SummaryComparability of r
Page 5 and 6: 1 CONTEXTUnder Regulation EC No 882
Page 7 and 8: processed in a single process or se
Page 9 and 10: 7 LABORATORY TESTING7.1 Number of t
Page 11 and 12: Other:Testing conditions should be
Page 13 and 14: The simulant from the first and sec
Page 15 and 16: The sets of test specimens should t
Page 17 and 18: For articles that:- are fillable an
Page 19 and 20: April 2004 on official controls per
Page 21 and 22: Annex 1 - Primary aromatic aminesTh
Page 23 and 24: 1 PROTOCOL A BY LC-MS1.1 PrincipleT
Page 25 and 26: litre of methanol.Mobil phase B: Pr
Page 27: 1.3.4 Quantification of analyte lev
Page 32 and 33: Gradient (linear):Time % A % B0.0 m
Page 34 and 35: 2.4.2 Detection limitsDL estimated
Page 36 and 37: 3.2.1.13 4,4'-Methylenedianiline (4
Page 38 and 39: Samples) the concentration (C) of t
Page 40 and 41: Appendix A: UPLC ConditionsColumn:A
Page 42 and 43: 4.2 Materials and chemicalsNOTE: Re
Page 44: Dwell volume0,9 ml4.3.3 HPLC calibr
Page 48 and 49: Table of contents1 PROTOCOL A......
Page 50 and 51: Repeat the procedure to obtain a se
Page 52 and 53: prepared stock solutions shall be c
Page 54 and 55: food simulant, depending on the typ
Page 56 and 57: European CommissionEUR 24815 EN - J
Page 58: The mission of the JRC is to provid

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