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

Abstract

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.

Keywords:

• migration
• food contact materials
• migrants
• foods
• contaminants
• packaging
• dry foods
• Tenax
• analytical methods
• interlaboratory
• comparisons
• validation

Acknowledgments

While previous methods described in the official methods available (CEN 1999, CEN 2003) used 4 g, which was fairly costly, the present methods reduced the amount needed to 1 g, thus reducing costs while retaining an efficient test performance. The authors wish to acknowledge the laboratories that participated in this exercise: Czech Republic – NIPH-NRL for Food Contact Materials and for Articles for Children Under 3 Years Old, National Institute of Public Health (SZU’); Denmark – Department of Food Chemistry, National Food Institute Technical University of Denmark; Estonia – Health Protection Inspectorate, Central Laboratory of Chemistry; Finland – Finnish Customs Laboratory; France – SCL Laboratoire de Bordeaux-Pessac; Germany – Bundesinstitut für Risikobewertung (BFR) (Federal Institute for Risk Assessment); LAV Sachsen-Anhalt, Fachbereich Lebensmittelsicherheit, Halle; and Bayerisches Landesamt für Gesundheit und Lebensmittelsicherheit, Erlangen; Ireland – Public Analyst Laboratory, Sir Patrick Duns Hospital; Luxembourg – Laboratoire National de Santé, Division du Controle des Denrées Alimentaires; Poland – Laboratory of Department of Food and Consumer Articles Research, National Institute of Hygiene; Portugal – ESB-SE (Portuguese Catholic University – Biotechnology College – Packaging Department); Slovenia – National Institute of Public Health of Republic of Slovenia, Department of Sanitary Chemistry; Spain – Centro Nacional de Alimentación, Agencia Espanola de Seguridad Alimentaria y Nutrición (AESAN); the Netherlands – Food and Consumer Product Safety Authority (VWA), Ministry of Economic Affairs, Agriculture and Innovation; and UK – Food Environment Research Agency (FERA).

Funding

This work was supported by the European Commission under the work programme of the EURL-FCM administrative arrangement AA SANCO /2012/FoodSafety070-FoodContactMaterials.