Effect of the Nature and Concentration of Phthalates on Their Migration from PVC Materials Under Dynamic Simulated Conditions of Mouthing

Polyvinylchloride (PVC) has been a very common material for the production of toys. It generally is manufactured with an addition of additives such as plasticisers to improve its functionality and facilitate its production process. PVC that can contain up to 50% by weight of plasticisers (Simoneau et al., 2001). Among plasticisers, 90% of the most commonly used to soften polymers for toys production are constituted by phthalates, such as diisononyl phthalate (DINP). The purpose of this study was to investigate the influence of the relative concentration of percentage of phthalates and nature of phthalates on their release in standard conditions. To obtain a suitable but rapid method of analysis, experiments were performed to study the effects on the modification of a standard operation procedure (SOP) previously validated at the EU level by JRC Ispra. A single extraction with a sufficient large volume of cyclohexane thus could be used instead of two extractions with a smaller volume of cyclohexane and resulted in more rapid yet reliable method. The final method is described in Annex 1 of this report. Samples of soft PVC were industrially produced especially for this study. Standard PVC disks with various percentages of di-isononyl phthalate (DINP), di-isodecyl phthalate (DIDP), di-ethyl-hexyll phthalate (DEHP), benzylbutyl phthalate (BBP) dibutylphthalate (DBP) or a binary mixture DINP/DBP in various proportions were prepared. 30 different types of disk were produced and tested. The disks were analysed for contents, homogeneity and sets were subjected to migration experiments of the various phthalates under dynamic conditions using the previously validated SOP with some modifications. The release from samples with a systematic manufacturing process and containing different phthalates at different concentrations showed correlations to their concentrations. Since previous studies using commercial toys had no showed such specific trends, these results suggest that the production process of toys may be an important issue with respect to release properties. The release of DEHP BBP and DBP tended to show a more linear correlation to the concentration, whereas for DINP, DIDP, DEHP and release the plasticiser showed non linear tendencies and saturation of release for high formulation contents.JRC.I.2-Chemical assessment and testin

Suitability of new sources of olive oil intended to be used as simulant D in migration testing

Regulation EC/882/2004 on Feed and Food Controls establishes the JRC as Community Reference Laboratory for Food Contact Materials (CRL-FCM). The Regulation requires a supporting network of European National Reference Laboratories (NRLs). This Regulation supports the harmonised enforcement of food legislation including food contact materials and the creation of a reference laboratory system operated by the JRC to systematically exchange and assess information on emerging issues related to chemicals released from food contact materials. The Council Directive 85/572/EEC of 19 December 1985 lays down the list of simulants for overall and specific migration testing, to be used for testing migration of constituents of plastic materials and articles intended to come into contact with foodstuff. This Directive lists the appropriate simulants to be used in migration tests with a particular foodstuff or group of foodstuffs. Within simulants, simulant D is rectified olive oil that has to satisfy characteristics such as acidity, peroxide index, iodine index, refractive index. Until 2005 rectified olive oil with documented appropriate technical specifications was commercially available from the company Pira International (UK). However commercial production stopped, and other potential sources available (Korea Japan, Sigma) did not necessarily provide specifications documented specifically for use as ¿simulant D¿. Since the oil specifications set in the EU legislation are crucial, both for compliance testing but also in the frame of an ISO accreditation for migration in oil, NRLs suggested the CRL-FCM to investigate specifications potential sources of olive oil to develop a source of simulant D for their purposes. The purpose of this study was to: ¿ Find potential suppliers for rectified olive oil ¿ Evaluate characteristics of oil on batch samples ¿ Select one supplier to purchase a lot of adequate defined specifications ¿ Establish the adequacy and homogeneity of the oil of a 500L lot ¿ Confirm the evaluation by independent analyses and certification by a specialised accredited institution for those specifications. The results demonstrated the feasibility of at least one source of olive oil, which was then provided to the National Reference Laboratories as a deliverable of the workprogramme 2007.JRC.I.5-Physical and chemical exposure

Report of the interlaboratory comparison organized by the Community Reference Laboratory Food Contact Material: Plasticisers in Gaskets and Oil

The Institute for Health and Consumer Protection (IHCP) of the European Commission¿s Directorate-General Joint Research Centre hosts the Community Reference Laboratory for Food Contact Materials (CRL-FCM). One of its core tasks is to organize interlaboratory comparisons (ILCs) among appointed National Reference Laboratories (NRLs). This report presents the results of the first ILC of the CRL-FCM which focused on the determination of Plasticisers content in PVC Gasket and in Oil matrix. The test materials used in this exercise were virgin gasket lids coming from industrial sources for the proficiency exercise part A. For the second part of the exercise an industrial source of sunflower oil was used and spiked with several plasticisers by the CRL-FCM. There were 41 participants to whom samples were dispatched 34 of which submitted results for at least 1 analyte-material. 21 laboratories reported results for more than 10 analyte-material combination out of 14 required. The homogeneity studies were performed by the CRL-FCM laboratory. The assigned value and its uncertainty for part A, virgin gaskets, were obtained after applying the robust statistics to the results obtained from the participants. The assigned values for part B, oil samples, were those obtained based on formulation, from the gravimetric measurements used to spike the material. The uncertainty of the assigned values for oil samples was calculated combining the uncertainty of the spiking procedure with a contribution for the between-bottle homogeneity. Participants were invited to report four replicates measurements. This was done by most of the participants. Laboratory results were rated with z and z¿ scores in accordance with ISO 13528 [1] Standard deviations for proficiency assessment (also called target standard deviations) were set based on Horwitz equation for substances in the two oil samples. For the plasticisers in the two gasket samples the target standard deviation was set by the organizers to 15% in order to fulfil the required criteria for sufficient homogeneity of the sample within the lots.JRC.I.2-Chemical assessment and testin

Training workshop "Safety of food contact materials: Technical Guidelines for Testing Migration under Regulation EU No 10/2011"

This report outlines the results of the Workshop Technical Guidelines on Migration Testing under Regulation EU No 10/2011JRC.I.1-Chemical Assessment and Testin

Stability of Selected Plastic Additives in Food Simulants

Within the framework of the AIR3 PL94 2360 EU-project, the stability of 3 plastic additives in 3 EU aqueous food simulants (distilled water, 3% acetic acid, 15% aqueous ethanol), one fatty simulant (olive oil) and in the alternative simulants 95% aqueous ethanol and isooctane were studied under various time-temperature conditions. The tested additives were bis(2-ethylhexyl) adipate (DEHA), bis(2-ethylhexyl) phthalate (DEHA) and octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate (Irganox 1076). The various test conditions included 10 days at 40 C, 1 hour at 100 C for all aqueous simulants, 10 days at 40 C and 1 hr 175 C for the olive oil, and 2 days at 20 C and 3 hr at 60 C for the isooctane simulant. Following the time-temperature exposure, the additive samples were solvent extracted from aqueous simulants using exane (1:1). In the case of isooctane simulant, the samples were analysed directly from the simulant. The oil samples were extracted by acetonitride in the case of DEHA and DEHP, and using size exclusion in the case of Irganox 1076. The extracts of DEHA, DEHP and Irganox 1076 samples exposed to various heat conditions as well as unexposed spiked controls and blanks were analysed by Gas Chromatography on a non polar 5% phenyl methyl polysiloxane capillary column. The results showed that DEHA, DEHP and Irganox 1076 were stable at 40 C and 100 C in ethanol or acid containing aqueous simulants. The various additives were also stable in olive oil as well as in the alternative fatty simulant isooctane. Studies on the stability of such additives used in food packaging are designed for regulatory purposes as an aid to decide whether the legislation should regulate limits for plasticisers based on a quantity in the food packaging itself or based on an ingested dose by the consumer.JRC.(EI)-Environment Institut

Effects of Capillary Columns on Long Term Routine High Temperature Analysis of Intact Triglycerides.

Abstract not availableJRC.(EI)-Environment Institut

Detection and Quantification of Cocoa Butter Equivalents in Chocolate Model Systems. Analysis of Triglyceride Profiles by High Resolution GC

The detection of vegetable fats added to coca butters in chocolateformulations was investigated in model mixtures. Cocoa butters varying inorigins, crop and treatment were analysed alone and combined at levels of 5, 10, 15 or 20% to a variety of cocoa butter equivalents. Triglyceride profiles were obtained by high resolution GC. The areas of the major triglycerides present were plotted one vs. the other. The plots percentages of specific triglycerides showed the capabilityto detect vegetable fats added to cocoa butters in these model systems, and quantification of the addition could be done down to a 5% level on a cocoa butter basis. The detection was most difficult in the case of the addition of illipe fat and the quantification could not be done below 10%. The results suggest that in chocolate, which contains 20-25% cocoabutter, this detection system is able to reach down to 1-2%, thus well below the proposed 5% regulatory level.JRC.I-Institute for Health and Consumer Protection (Ispra

Comparison of Classical and Alternative Extraction Methods for the Quantitative Extraction of Fat from Plain Chocolate and the Subsequent Application to the Detection of Added Foreign Fats to Plain Chocolate Formulations.

Abstract not availableJRC.I-Institute for Health and Consumer Protection (Ispra

Time-Temperature Study of the Kinetics of Migration of BADGE (Bisphenol-A-Diglycidyl-Ether) into Fatty Medium.

Abstract not availableJRC.I-Institute for Health and Consumer Protection (Ispra

Spatial Distribution Patterns of Metals in the Surface Sediments of Lake Orta (Italy)

Abstract not availableNA-NOT AVAILABL