European Regulations For Multilayer Food Contat Materials Dr. Hermann Onusseit Henkel KGaA Düsseldorf, Germany ABSTRACT Artiles and failities whih ome into ontat with food are subjet to speial demands. This applies to proessing and also to transport and warehousing of food. These artiles are requested to not influene the food they ontat, neither toxiologially i. e. no health threat for the end-user, nor may they hange the omposition of the food and the properties like smell, taste and look. Most materials that ome into ontat with foodstuffs onsist of different parts or omponents, whih together form an artile, eg, a pakage. Often adhesive is used for holding together the parts. In a multi-layer pakage, those layers not in diret ontat with foodstuff may not be negleted, beause their onstituents may migrate through the food-ontat layer. While there are already European regulations for plastis, for other omponents like printing inks or adhesives a preparation is intensively disussed. The establishment of a positive-list system for those omponents will require very muh time and money and this surely annot be aomplished for all formulation omponents used today. Thus in the future a number of formulations may no longer be legal for food ontat materials. A positive-list system absolutely requires an individual ompliane hek with speifi migration limits. It has to be onsidered that onventional migration test proesses are time-onsuming and ostly and that there are no analytial methods for many omponents yet. As a onsequene the only possible and useful way is a speifi testing onept by a ombination of extration and migration tests and mathematial modelling, that guarantees the safe use of these omponents in multilayer food ontat materials, and whih an be utilized ost-effiiently by the industry, espeially by small and medium-sized enterprises. INTRODUCTION Food ontat materials are used in the prodution of artiles intended to ome into ontat with foodstuffs, like utlery, dishes, proessing mahines, ontainers and above all pakaging [Fig. 1]. This applies to both the proessing of food and to its transport and warehousing. The term also inludes materials and artiles that are in ontat with water intended for human onsumption, but it does not over fixed publi or private water supply equipment. Food ontat artiles shall be safe and shall not transfer their omponents into the foodstuff in unaeptable quantities. These artiles are requested to not influene the food they ontat, neither toxiologially ie, they should not ause a health threat for the end user, nor may they hange the omposition of the food or its properties like smell, taste and appearane. THE EUROEAN AROACH On the European level two authorities deal with questions of food safety. One is the European Union and the other is the Counil of Europe. While the deisions of the European Union are obligatory for national legislations, those of the Counil of Europe are only a reommendation. THE EUROEAN UNION A first framework diretive on materials and artiles intended to ome into ontat with foodstuffs was adopted in 1976. It was replaed in 1989 by the Framework Diretive 89/109/EEC. This basi law for food ontat artiles was laid down in the Counil Diretive of 1 Deember 1988, onsolidating the laws of the member states relating to materials and artiles intended to ome into ontat with foodstuffs. The framework diretive applies to all materials and artiles intended to ome into ontat with foodstuff. Detailed explanations about how these prinipal demands should be transformed are desribed in speifi regulations within the framework diretive. Hene in the past 15 years some speifi diretives have been prepared, eg, for plasti materials, the so-alled lasti Diretive, first published in 1990 (90/19/EEC). The urrent version of the lasti Diretive is from 00
(00/7/EC). Others exist for regenerated ellulose films, eramis, and vinyl hloride monomer. Due to tehnologial development it was neessary to adjust this framework diretive in 004. Hene on 7 Otober 004 the new Framework Regulation (EC) 1935/004 was enated and published in the European Offiial Journal on 13 November 005. In ontrast to a diretive, whih has to be onverted after publiation by the European Union within a ertain period by the individual member states into national law, a regulation is automatially onverted into the national law of all EU ountries twenty days after publiation. In this new framework regulation also some new artiles and groups of substanes were inluded for whih speifi regulations should be prepared. Some materials and artiles to whih future speial diretives or regulations will apply are ative and intelligent materials and artiles, adhesives, paper and board, printing inks, rubber, glass, metal and alloys, wood, ork, textiles, waxes, varnishes and oatings and ion-exhange resin [Fig. ]. The regulation set some general requirements that must be met by all food ontat materials: All materials and artiles must be manufatured aording to Good Manufaturing ratie (GM) so that they do not transfer their onstituents to foodstuffs in quantities whih ould endanger human health or "bring an unaeptable hange in the omposition of the foodstuff or a deterioration in the organolepti properties". In artile 3 the following general requirements are mentioned. Materials and artiles, inluding ative and intelligent materials and artiles, shall be manufatured in ompliane with good manufaturing pratie so that, under normal or foreseeable onditions of use, they do not transfer their onstituents to food in quantities whih ould: (a) endanger human health; or (b) bring about an unaeptable hange in the omposition of the food; or () bring about a deterioration in the organolepti harateristis thereof. The transfer of omponents from the food ontat materials into food is alled migration. To ensure the protetion of the health of the onsumer and to avoid alteration of the foodstuff, two types of migration limits have been established in European law. For the first time these numerial values appeared in the Commission Diretive of 3 February 1990 relating to plasti materials and artiles intended to ome into ontat with foodstuffs: an overall migration limit (OML) of 60mg (of substanes)/kg (of foodstuff or food simulants) that applies to all substanes that an migrate from the food ontat material into the foodstuff and a speifi migration limit (SML) whih applies to individual authorized substanes and is fixed on the basis of the toxiologial evaluation of the substane. The SML is generally established aording to aeptable daily intake (ADI) or tolerable daily intake (TDI). These values formerly were set by the Sientifi Committee on Food (SCF) and today are set by the European Food Safety Ageny (EFSA). To set the limit, it is assumed that every day throughout his/her lifetime, a person of 60kg eats 1kg of food paked in plastis ontaining the relevant substane at the maximum permitted quantity. The urrent approah for the authorization and ontrol of substanes used in food ontat materials is onsidered to be autious in relation to the estimation of potential exposure of the onsumer to these substanes. Approahes are being disussed whih take into better onsideration the atual exposure of the onsumer to food ontat materials in risk assessment. The use of mathematial modelling for predition of migration, whih an redue the amount of tests to be undertaken, has been reently introdued into the legislation. ratial examples for the appliation of this new onept are desribed in the ratial Guide. THE COUNCIL OF EUROE Even though there is no formal agreement between the European Union and the Counil of Europe onerning food ontat materials, there are important and numerous ontats between the servies of the Health & Consumer rotetion Diretorate-General and the Counil of Europe in this field. The Counil of Europe has prepared a number of douments, whih are used as basis for many national regulations in Europe.
The Committee of Ministers has adopted the following resolutions: Resolution A (89) 1 on the use of olourants in plasti materials oming into ontat with food Resolution A (9) on ontrol of aids to polymerisation for plasti materials and artiles Resolution A (96) 5 on surfae oatings intended to ome into ontat with foodstuffs Resolution A (97) 1 on ion exhange and adsorbent resins used in the proessing of foodstuffs (superseding Resolution A (89) ) Resolution A (99) 3 on siliones used for food ontat appliations Resolution A (00) 1 on paper and board materials and artiles intended to ome into ontat with foodstuffs Framework Resolution A (004) 1 on oatings intended to ome into ontat with foodstuffs Resolution A (004) on ork stoppers and other ork materials and artiles intended to ome into ontat with foodstuffs Resolution A (004) 3 on ion exhange and adsorbant resins used in the proessing of foodstuffs Resolution A (004) 4 on rubber produts intended to ome into ontat with foodstuffs Resolution A (004) 5 on siliones used for food ontat appliations resent ativity programme of the Committee of experts: List of substanes on paper and board produts intended to ome into ontat with foodstuffs (onerning Resolution A (00) 1); Draft guidelines on the safety evaluation of food ontat paper and board substanes; Draft resolution on printing inks, primers, oloured laquers and overprint varnishes applied to the nonfood ontat surfae of food pakaging and artiles intended to ome into ontat with foodstuffs; Guidelines on lead leahing from glass tableware into foodstuffs; Guidelines on tissue paper kithen towels; All the above-mentioned topis will inlude toxiologial and tehnologial speifiations and limits as well as inventory lists of hemial substanes used for the manufature of these substane groups. MULTILAYER FOOD CONTACT MATERIALS Most materials that ome into ontat with foodstuffs onsist of different parts or omponents, whih together form an artile, eg, a pakage. Often adhesive is used for holding together the parts. In a multi-layer pakage, those layers not in diret ontat with foodstuff may not be negleted, beause their onstituents may migrate through the food-ontat layer. This thought was desribed for the first time in the so-alled "Super Regulation". The driving idea in writing the "Super Regulation" (former "Super Diretive") was to ollet in one text the rules set out in all the diretives related only to plasti materials and artiles ie, Commission Diretive 00/7/EC and its amendments, onsolidation of 8/711/EEC and its two amendments, 93/8/EEC and 97/48/EC; 85/57/EEC; and the three vinyl hloride monomer diretives, 78/14/EEC, 80/766/EEC and 81/43/EEC. This should be onsidered as an attempt to prepare a future ommission diretive on all types of plastis. As usual, the regulation or diretive ontains only general priniples of the tehnial rules suh as modelling, funtional barrier et. Details and guidane will be introdued at CEN level or in the ratial Guide. To give an idea of the repartition of the rules, some examples or referenes to existing douments are given in the draft of the "Super Regulation", suh as the extension of the rules to multilayers omposed of different materials and the introdution of the new onept of "funtional barrier". It has to be noted that the layer ating as "funtional barrier" may be either authorized by the diretive and listed together with the onditions of its validity, or used without any authorization by the manufaturer provided that the written delaration of ompliane mentions the substanes not subjet to an authorization proedure. A multilayer plasti food ontat material shall omply with the following rules: Any layer shall be manufatured
from substanes mentioned in a Community list subjet to their restritions. In absene of a Community list, substanes whih appear in a national list from a European ountry may be used provided they omply with artile 3 of Resolution (EC) 1935/004. In the absene of these lists, only substanes in amounts whih, in the pratial use of the final materials or artiles, an be proved to omply with artile 3 of Resolution (EC) 1935/004 may be used. These substanes are hereinafter referred to as "Listed food ontat substanes". The finished artiles shall omply with the OML, the SML and the other speifi restritions of the substanes ontained in the different layers; eah layer maintains its own speifiations. A "Funtional Barrier" is a barrier onsisting of one or more layers that ensures that migration of adhesive omponents does not exeed their SML, and whih redues the migration of these omponents, their reation produts, and impurities into food to a "non-detetable" level when subjeted to a validated test method. For the purpose of ontrol, "non-detetable" means that a substane annot be deteted at a onentration appropriate for the nature of the substane, but in no ase exeeding 0.01 mg/kg. This detetion limit, whih is urrently disussed, applies to groups of struturally related ompounds, eg, isomers. DECLARATION OF COMLIANCE To guarantee the onformity of the used materials the Framework Regulation (EC) 1935/004 demands in artile 16 the preparation of a delaration of ompliane. This thought is desribed in the draft of the Super Regulation in detail. The written delaration of ompliane shall permit an easy identifiation of the materials or artiles for whih it is issued and shall be reviewed periodially. It shall ontain the following information: Identity of material or artile; its range of appliation; and the onfirmation that the material or artile omplies with the requirements of the European diretives and, when appropriate, with national law. When a funtional barrier is used in a multilayer material, the following additional information shall be provided: The identity of the substanes of the funtional barrier, the date of latest use of the material or artile; and the maximum heat treatment (temperature and time) for the artile. At eah stage of manufature, proessing, and distribution an appropriate tehnial doumentation able to demonstrate the ompliane of the material, artile or substanes with the relevant provisions shall be available. This doumentation, hereinafter alled "Supporting Douments", shall ontain the desription and the results of the analysis arried out to demonstrate the ompliane of the material and artile, and in partiular the ompliane with quantitative restritions in the use of the substanes suh as OML, SML et, plus the requirements of the layer(s) onstituting a funtional barrier, and the requirements set out in Artile 3 of Framework Regulation (EC) 1935/004 related to the substanes migrating in detetable amounts and whih are not listed in positive lists. ADHESIVES IN MULTILAYER FOOF CONTACT MATERIALS For the prodution of many artiles that are intended to ome into ontat with foodstuffs, adhesives are used. There are non-pakaging appliations like refrigerators, mirowave ovens, kithen furniture or orks for beverage bottles, but of speial importane is the use of adhesives in the prodution of mass artiles like pakaging [Fig. 3]. akaging protets goods against damage and loss. In addition, pakaging is essential for safe distribution and warehousing [Fig. 4]. Today s variety of produts would not be possible without modern pakaging. The usefulness of modern pakaging an be demonstrated very impressively with food. While modern pakaging has eliminated the risk of ontamination of food by bateria or insets almost ompletely, the lak of suitable pakaging and distribution results in dramati losses due to deterioration. A omparison between industrialized and developing ountries shows the impat of proper pakaging on losses of food during storage and transport. Whereas in the industrialized ountries only about 5% of all food deays thanks to the sophistiated pakaging tehnology, in developing ountries it is almost two thirds [Fig. 5]. For the prodution of many of these pakagings, today a vast number of adhesive systems are available. Appliations inlude laminations of flexible films to foil, paper/ardboard film ombinations, rigid multi-layer plasti pakaging, saks and bags, and labelling usually without, but sometimes also with diret food ontat. The evolution in materials and proesses led to an intensive development of pakaging adhesives in reent
deades, so that today there are tailor-made pakaging adhesives for all kinds of appliations and performane demands. The adhesives that are used for the prodution of these artiles are requested to fulfil all tehnial requirements as well as the requirements of the European diretives and regulations for materials and artiles intended to ome into ontat with foodstuffs. Adhesives are not yet treated as an individual regulated group, so that the European regulation of adhesives still is not harmonized. However in 00 the European Commission (DG SANCO) started disussions to regulate adhesives. A first hearing about this subjet took plae in Brussels in 001. The urrent draft (Rev. 5. dated 1 July 004) of the so-alled "Super Regulation" intends to inlude the migration ontributions of the adhesives used in multilayer onstrutions, but without mentioning a speifi regulation. In addition adhesives are mentioned as a group of substanes to be regulated in the appendix 1 of the new Framework Regulation (EC) 1935/004. In disussions with FEICA several different approahes were prepared. From today s point of view the following possibilities for future regulations of adhesives an be imagined: 1. Inlusion in the positive-list system of the lasti Diretive 00/7/EG or in the suession regulation of the lasti Diretive, alled "Super Regulation", whih is urrently disussed.. A speifi diretive for adhesives with a speial positive list for adhesives. 3. The industry works out its own onept whih has to be aeptable by the enforement, and whih ensures the ompliane of the produts regarding Art. 3 of the Framework Regulation (EC) 1935/004 ), namely the general demands (not to endanger human health). OSITIVE-LIST SYSTEM The positive-list system means that all raw materials and additives used for prodution of an adhesive have to be listed in a European guideline dealing with adhesives for food ontat materials (00/7/EG, "Super Regulation" or a speifi diretive). This proedure offers the advantage that finally all substanes used have to be evaluated by the European Food Safety Ageny (EFSA) and offiially authorized. If neessary, limits have to be set in the European Adhesive Regulation. Some of the raw materials and additives used for adhesives are also used for plastis and so are already evaluated. However it has to be onsidered that short-hain polymers, suh as are used in those adhesives whose visosity is ontrolled by the length of the polymer hain, are now defined as polymer additives and are not regulated by the list of monomers and raw materials, but must be authorized speifially. However, most raw materials used for the prodution of adhesive formulations are not used in the already regulated prodution of plasti materials. These, as well as the short-hain versions of approved plastis, have to pass through an approval proedure before they are inluded in the list. For this, migration and toxiologial studies based on the extent of migration are neessary. Depending on the knowledge of the raw materials these studies an require a lot of effort and be expensive. To get all neessary data for migration tests approximately 3,000 50,000 EUR and for the toxiologial dossier approximately 50,000 500,000 EUR (range based on migration levels) are estimated. In addition, reations and by-produts have to be measured and taken into aount. Depending on their amount and omposition, migration toxiologial data an also beome neessary for them. It is obvious that an inlusion in the positive-list system of all substanes used in adhesives would be an enormously time-onsuming and expensive proess. To illustrate this amount of time one should look at the development of the positive list for plasti monomers. When the lasti Diretive 90/18/EEC was established, monomers and other raw materials that were used before 1990 for the prodution of plastis for food ontat, but whih had not yet been evaluated by the Sientifi Committee for Food (SCF), were inluded in a B list of temporarily-usable substanes pending a deision on inlusion in the positive list (Setion A). This B list will presumably be anelled by 31 Deember 007, meaning that it will have taken 17 years until the last old monomers and other starting substanes have been evaluated and inluded in the A list of the approved monomers, or deleted. It is assumed that some of the raw materials used for adhesives (and espeially the additives) will get speifi
migration limits based on toxiologial evaluation. The ompliane with migration limits has to be ontrolled on the finished food ontat material. As adhesives onsist of many omponents a migration test by the old proedure would be very expensive and time-onsuming. For many or for most of the omponents today there are no, or at least no validated, analytial measurement methods. THE INDUSTRY S OWN CONCET In ontrast to the materials of whih food ontat artiles like pakages prinipally onsist, adhesives are usually only a minor omponent. The tonnage of adhesives is but a minor perentage of the tonnage of, for example, paperboard and plasti. Thus the pressure for adhesive raw material produers to invest time and money in the approval of raw materials is limited, and beause of this the adhesive industry will lose a substantial number of raw materials. The onsequene ould be that some of today s adhesive formulations will not onform to the food regulations anymore and therefore be forbidden for these appliations. The alternative to the positive-list system would be to prepare a praxis-orientated testing onept to guarantee the safe use of adhesives in multilayer food ontat materials. This test ould be developed by the adhesive industry, inluding small and medium-sized enterprises, ost-effiiently and without ompromise to onsumer protetion requirements and thus to their own produt image. Suh a onept finally should be given to the European authorities to be written in a legal format. Most likely, the general priniples would be embedded into a European regulation. The neessary details would be laid down in the so-alled ratial Guide for food ontat materials of the Commission. The pratial guide is based on the fat that adhesives are usually between two other materials, ie, that there rarely is diret ontat of adhesive and foodstuff. Hene the omponents of the adhesives annot migrate into the foodstuff diretly, but have to migrate through a barrier layer [Fig. 6]. For the first time, this view has been desribed in the so-alled "Super Regulation", too. The pratial guide also takes into aount the relatively small quantity of adhesive ompared to the material that forms the food-ontat artile itself, eg, slim glue lines of folding boxes [Fig. 7]. The evaluation of the migration of adhesive omponents into foodstuff ould be based on the priniple of the soalled "Funtional Barrier" (FB), whih will presumably be onsidered within the regimentation of the "Super Regulation". The basi idea behind the FB priniple is that the food ontating layer(s) (of a multilayer) may at as a barrier for migration of adhesive omponents (ie, a funtional barrier). The performane of a funtional barrier depends on the properties of the food ontating layer and the migrating substane. As a onsequene, substanes that are immobilized in the adhesive or that annot migrate into the food beause of the funtional barrier properties of the interior layers under the presumed use onditions, an be omitted from this onept of approval. Then a toxiologial evaluation would only be neessary for those substanes that an migrate in signifiant or large amounts. In reative systems, by-produts are formed, often of unknown omposition. Usually it is very diffiult to reeive suffiiently detailed information about the omposition and purity of raw materials from raw material suppliers. This should be onsidered in the test onept by utilizing pratial validated sreening methods on omponents able to migrate. The test should be usable even when one does not have exat knowledge of all individual substanes used in the adhesive formulation. Tests of migration and migration kineti tests for barrier materials are very time-onsuming and expensive. Usually, the adhesive exists in a very thin layer, and the amount of omponents able to migrate is small, so that suh sophistiated migration tests often are not neessary. The test onept hene should be a fast, ost-effetive, and relatively easy method of determining ompliane. This should be ahieved by a ombination of extration tests to determine the potential of omponents able to migrate, mathematial modelling, and but a few verifying migration tests of the finished food ontat materials. Conlusions should be drawn from a tested system with defined layers and layer thiknesses about the ompliane of other systems with the same adhesive, without ausing the need for new tests. Regardless of whih of these approahes will be inorporated into the regulations, in the future the European idea,
whih is haraterized by onsumer and environmental protetion, will lead to a lear expansion of the neessary doumentations and surveys of adhesives and adhesive raw materials used for food ontat materials. Espeially for raw materials it will be neessary to dislose many ingredients, so that proessors an exeute orresponding surveys. The adhesive industry, too, will have to give muh more information to its ustomers, so that ustomers an ensure the ompliane of their artiles with the European food ontat material regulation. MATHEMATICAL MODELLING Adhesives are onsiderably more omplex systems than mono plastis, so that the modelling methods used for plastis until now annot be simply transferred to the testing of adhesives. Beause of this there is yet no sientifially stable basis for simplified testing of adhesives. Different researh institutes have prepared the ground in this field of researh and from these preparations suh a onept an be developed. The mathematial modelling of migration [Fig. 8] from mono plastis and the estimation of diffusion oeffiients as proof (iringer model) is validated for many plastis and has been inluded as a possibility to test the ompliane in the European lasti Diretive 00/7/EG (artile 8/4) and ratial Guide. The model has been published among others as a guide in the ratial Guide for Food Contat Materials of the European Commission and as a CEN Report. It has been extended to the appliability on multilayer materials in onnetion with a reently finished researh projet. To prepare the neessary sientifi data a European projet is being planned by several researh institutes. The projet will be assisted by FEICA and by a number of national European adhesive assoiations, as well as by small and medium-sized adhesive manufaturers. SUMMARY Without multilayer food ontat materials modern life would not be possible. While there are already European regulations for plastis, for other omponents like printing inks or adhesives a preparation is intensively disussed. The establishment of a positive-list system for those omponents will require very muh time and money and this surely annot be aomplished for all formulation omponents used today. Thus in the future a number of formulations may no longer be legal for food ontat materials. A positive-list system absolutely requires an individual ompliane hek with speifi migration limits. It has to be onsidered that onventional migration test proesses are time-onsuming and ostly and that there are no analytial methods for many omponents yet. As a onsequene the only possible and useful way is a speifi testing onept by a ombination of extration and migration tests and mathematial modelling, that guarantees the safe use of these omponents in multilayer food ontat materials, and whih an be utilized ost-effiiently by the industry, espeially by small and medium-sized enterprises. ACKNOWLEDGEMENTS The author would like to thank Bill Leah, Henkel Adhesives, Hayward, USA, for his valuable assistane.
Fig. 1 Food Contat Artiles Regulation of the European arliament and of the Counil on materials intended to ome into ontat with food: (EC) 1935/004 Annex 1: List of groups of materials and artiles whih may be overed by speifi measures Ative and intelligent materials and artiles Adhesives Ceramis Cork Rubbers Glass Ion-exhange resins Metals and alloys aper and board lastis rinting ink Regenerated ellulose Siliones Textiles Varnishes and oatings Waxes Wood Fig. Speifi Regulations Fig. 3 akaging
Fig. 4 Distribution with akaging % 70 60 50 40 30 0 10 0 The developed world Developing ountries Fig. 5 Loss of Food During Transport and Warehousing Adhesives Funtional Barrier Foodstuff / Simulant D A K A,FB D FB K FB,F Migration Fig. 6 Migration in Multilayer
Fig. 7 Adhesive Appliation Fig. 8 Migration Modelling (single layer) Fik s nd law σ = e n r z y x total k k z v y v x v z y x D t ( ) = =1,0, exp 1 1 1 1 n n n t L d q t D q d A m ρ L L K V V, / =