Optimisation of an analytical method and results from the inter-laboratory comparison of the migration of regulated substances from food packaging into the new mandatory European Union simulant for dry foodstuffs.

This paper presents the outcome of the development, optimisation and validation at European Union level of an analytical method for using poly(2,6-diphenyl phenylene oxide--PPPO), which is stipulated in Regulation (EU) No. 10/2011, as food simulant E for testing specific migration from plastics into dry foodstuffs. Two methods for fortifying respectively PPPO and a low-density polyethylene (LDPE) film with surrogate substances that are relevant to food contact were developed. A protocol for cleaning the PPPO and an efficient analytical method were developed for the quantification of butylhydroxytoluene (BHT), benzophenone (BP), diisobutylphthalate (DiBP), bis(2-ethylhexyl) adipate (DEHA) and 1,2-cyclohexanedicarboxylic acid, diisononyl ester (DINCH) from PPPO. A protocol for a migration test from plastics using small migration cells was also developed. The method was validated by an inter-laboratory comparison (ILC) with 16 national reference laboratories for food contact materials in the European Union. This allowed for the first time data to be obtained on the precision and laboratory performance of both migration and quantification. The results showed that the validation ILC was successful even when taking into account the complexity of the exercise. The results showed that the method performance was 7-9% repeatability standard deviation (rSD) for most substances (regardless of concentration), with 12% rSD for the high level of BHT and for DiBP at very low levels. The reproducibility standard deviation results for the 16 European Union laboratories were in the range of 20-30% for the quantification from PPPO (for the three levels of concentrations of the five substances) and 15-40% from migration experiments from the fortified plastic at 60°C for 10 days and subsequent quantification. Considering the lack of data previously available in the literature, this work has demonstrated that the validation of a method is possible both for migration from a film and for quantification into a corresponding simulant for specific migration.

Effect of ethanol on the sorption of four targeted wine volatile compounds in a polyethylene film.

The objectives of this study were to demonstrate that the presence of ethanol in a solution containing two esters and two aromatic alcohols has several consequences on the sorption of these compounds into polyethylene (PE) film. First, sorption of ethanol into the PE film occurred at the same time as water and reached 8 kg m(-3) using 12% v/v of ethanol. This sorption was associated with an increase in PE crystallinity, which may have prevented the sorption of volatile compounds despite their strong affinity with PE film, as evaluated by Hansen solubility parameters. Moreover, increasing the ethanol concentration increased the solubility of the four volatile compounds. In the case of aromatic alcohols, the sorption was decreased in the presence of ethanol as expected. In the case of esters, as their hydrolysis was substantial in the presence of water, the consequence was a higher sorption into the PE film in the presence of ethanol than in its absence. Nevertheless, the sorption also depended on the concentration of ethanol and the heterogeneity of the ethanol-water mixture as well as the presence of other volatile compounds, as in the case of 4-ethylphenol. In conditions simulating wine packaging, losses of volatile compound by sorption and by permeation estimated after only 5 days of contact varied between 0.08 and 25% for 2-phenylethanol and ethyl hexanoate, respectively.

Effect of concentration and relative humidity on the transfer of alkan-2-ones through paper coated with wheat gluten.

The transport properties of two methyl ketones, 2-heptanone and 2-nonanone, through a paper coated with a wheat gluten (WG) solution were studied as a function of aroma compound concentration differential and relative humidity. Whatever the conditions, coating improved the aroma barrier properties of the paper. Whereas permeability of 2-nonanone through WG coated paper was not affected by the concentration differential, a high concentration of 2-heptanone induced a permeability increase, which can be explained by a slight plasticization effect of this compound. The moisture content of the films markedly affected the barrier properties depending on the aroma compound. For 2-heptanone, the most polar compound, the increase of permeability with relative humidity was related to the increase of diffusivity and solubility coefficient of this compound. With 2-nonanone, permeability and diffusivity coefficients strongly decreased with the increase of moisture content. This decrease could be linked to the hindrance in diffusivity of the less polar compound induced by the presence of water molecules. The different behavior in permeation properties seems to be related to the hydrophobic nature of the aroma compound. At intermediate and high humidity levels, coated papers are found to have better aroma barrier properties than LDPE films.