Determination of the overall migration from silicone baking moulds into simulants and food using 1H-NMR techniques

Ruediger Helling (1) , Anja Mieth (2) , Stefan Altmann (3) , Thomas Joachim Simat (2)

1 Landesuntersuchungsanstalt für das Gesundheits- und
2 Food Chemistry [Dresden]
3 Zentrale Analytik

37 samples of different silicone baking moulds were characterized concerning potential migrating substances using 1H-NMR, RP-HPLC-UV/ELSD and GC techniques. In all cases cyclic organosiloxane oligomers with the formula [Si(CH3)2-O]n have been identified (n = 6...50). Additionally, linear, partly hydroxyl-terminated organosiloxanes HO-[Si(CH3)2-O]n-H (n = 7...20) have been found in 13 samples. No other substances than siloxanes could be observed, meaning the migrants mainly consist of organopolysiloxanes. Based on this knowledge, a 1H-NMR quantification method for siloxanes was established working both for analysis of simulants and foodstuffs. Validation data of the 1H-NMR method gave a suitable performance: limit of detection 8.7 mg kg-1 oil, coefficient of variation 7.8 % (1.0 mg kg-1 food). Further experiments implied migration studies with simulants (olive oil, isooctane, ethanol (95 %), Tenax) as well as different preparation of cakes. Siloxane migration into cake was only slightly decreasing from 1st to 10th experiment with a significant dependence on fat content. Thereby migration values never exceeded an amount of 21 mg kg-1 (3 mg dm-2) and were therefore well below the overall migration limit of 60 mg kg-1 (10 mg dm-2). Migration behaviour into simulants differs completely from these results.

Mots clés: Life Sciences

Ruediger Helling, Anja Mieth, Stefan Altmann, Thomas Joachim Simat. Determination of the overall migration from silicone baking moulds into simulants and food using 1H-NMR techniques. Food Additives and Contaminants, 2009, 26 (03), pp.395-407. ⟨10.1080/02652030802520852⟩. ⟨hal-00577342⟩