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

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