Report FD 03/28 ACTIVE PACKAGING CURRENT TRENDS AND POTENTIAL FOR MIGRATION April-04

PROJECT INFORMATION Laboratory Report Number: Author: Date: Project title: Sponsor: FD 03/28 L Castle April 2004 Active packaging current trends and potential for migration Food Standards Agency Aviation House 125 Kingsway London WC2 6NH A03039 K6AD FLN 7576 L Castle 1. 2. 3. 4. Dr Barnes (FSA) (x5 + disk) CSL Library Dr Dennis (CSL) Prof. Gilbert (CSL)

Sponsors Project Number: CSL Project Number: CSL File Reference: Team Leader: Distribution:

CSL Sand Hutton York YO41 1LZ

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SUMMARY Active packaging is intended to influence the packed food. It is intended to change the condition of the packed food, to extend shelf-life or improve sensory properties while maintaining the freshness and the quality of the food. To do this, the packaging should absorb food-related chemicals or should release substances such as preservatives, antioxidants, flavourings or colours. For intelligent packaging, the food is intended to influence the packaging. The present UK market for such active or intelligent applications is small. It is concluded from the research described here that the major impact of any wider introduction of such packaging would fall on the sectors of direct food additives, food authenticity and food labelling. For these sectors, the recommendations of this report are: a) active ingredients (themselves or their by-products) which may become components of the food should comply with community provisions on food additives; b) active or intelligent packaging should not mislead the consumer; for example should not contradict whatever the consumer understands by fresh; c) such packaging should be suitable and effective for the intended use; d) it should comply with Directives 92/59/EEC (general product safety), as well as 89/109/EEC, and 87/357/EEC concerning misleading and unsafe claims, because for example if spoilage indicators are scavenged then food may have spoiled but the consumer cannot detect this. Any incidental chemical migration could be controlled using the existing legislative instruments provided that the Framework Directive was modified to encompass such packaging. For this sector, the recommendations of this report are: a) active or intelligent packaging should comply with the Framework Directive on food contact materials; b) such packaging materials should comply with the existing overall migration limit, excluding the active agent released intentionally; c) many of the active or intelligent systems rely on their active function (absorbing or releasing) operating through the gas phase. So testing for undesirable gas-phase migration should be considered. d) existing standardised test methods should in the main be applicable to testing active and intelligent packaging for migration, although some applications may required simulants that are not liquids for example a semisolid food simulant with liquid absorbed onto a carrier.

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Table of Contents 1. INTRODUCTION 1.1 Active packaging definition 1.2 Intelligent packaging definition 1.3 The scientific objectives of this work 2. THE PRESENT MARKET FOR ACTIVE PACKAGING IN THE UK 2.1 Wooden barrels for whisky 2.2 Meat pads and fish pads 2.3 Plastic fruit bags with an ethylene scavenger incorporated 2.4 Oxygen scavengers 2.5 Fungicides used in fruit wrappers 2.6 Microwave susceptors 2.7 Antimicrobial substances used to protect/preserve the food contact material 3. THE LIKELY FUTURE MARKET FOR ACTIVE PACKAGING IN THE UK 3.1 Absorbing systems 3.2 Releasing systems 3.2.1 Antimicrobial releasers 3.2.2 Antioxidant releasers CASE STUDY 1. Allyl Isothiocyanate from horseradish / mustard CASE STUDY 2. A photo-initiated oxygen-scavenging plastic 4. EVALUATE THE MIGRATION POTENTIAL FOR THE APPLICATIONS IDENTIFIED 4.1 Definitions 4.2 Intentional transfer (release) of substances to the food 4.3 Intentional removal (scavenging) of substances from the food 4.4 General observation on scavenging systems 4.5 General observations on active ingredients 5. EVALUATION OF THE ACTIPAKREPORT 6. APPLICABILITY OF EXISTING MIGRATION TEST PROTOCOLS 6.1 The test procedures and simulants already available 6.2 Applicability of existing migration test procedures 6.2.1 The physical nature of the food simulants commonly used 6.2.2 The chemical nature of the food simulants commonly used 6.2.3 The nature of the test apparatus employed 6.3 Standardisation of new analytical methods 7. REFERENCES

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1. INTRODUCTION There have been several recent reviews of active and intelligent food packaging upon which this report builds. They have covered both the technological aspects [1] [2] [3] as well as the legislative questions that these materials pose [4] [5] [6] [7] [8]. The state of the art was described most recently in the final report of a large EU-funded project Actipak [9]. 1.1 Active packaging definition A common way to define active packaging is to highlight what distinguishes it from so-called conventional (passive) packaging. Therefore, a working definition of active packaging is food packaging which has an extra function, in addition to that of providing a protective barrier against external influence. Active packaging is intended to change the condition of the packed food, to extend shelf-life or improve sensory properties while maintaining the freshness and the quality of the food In order to exert this function, active packaging must act in one of two possible ways Absorbers of food-related chemicals Scavengers of oxygen, water, carbon dioxide, ethylene, off-flavours like amines and aldehydes Emitters of food additives Releasing preservatives, antioxidants, flavourings, colours There is in fact a third category, which generally will not be discussed in detail further because they are intended to change only the physical properties of the food. However, an exception will be made for microwave susceptor materials, which will be described and discussed in later sections. These are materials that are intended to heat the food surface but which in operation can incidentally release thermal breakdown products of their constituents. Modifiers of physical properties Self-heating cans, widgets in beverage cans for foam formation It should be appreciated that such a clear distinction between active and passive packaging systems is simplistic. There is a gradation. For example, from (i) a barrier film which prevents gas exchange between a packed food and its environs, moving to (ii) a film made with a polymer blend that has selective permeability to different gasses and allows the food product to breathe, and then moving to (iii) a plastic film that has a chemical system built-in to the polymer to react with oxygen and so modify the pack atmosphere. The first is
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clearly passive, the third is clearly active, and the second (called EMAP equilibrium-modified atmosphere packaging) may be considered to be either active or passive because it clearly modifies the pack environment but permeability is a passive and not an active transport function. 1.2 Intelligent packaging definition Most of the technical, scientific and legislative problems that active packaging materials may pose are shared also by intelligent packaging materials. They have been defined as Concepts that monitor to give information about the quality of the packed food. Examples are indicators of: time-temperature storage history; carbon dioxide or oxygen status; spoilage status; and tamper-breakage information. Consequently for active packaging, the packaging is intended to influence the food for intelligent packaging, the food is intended to influence the packaging

1.3 The scientific objectives of this work The scientific problem that this project tackled was, therefore, how should these materials be authorised, regulated and tested [10, 11]? What special problems may be caused with respect to the quality and the safety of the packaged food? The project aimed to address 3 main areas. a) what future experimental migration work may be needed, if any; b) what changes to the CEN standard methods of migration testing are needed, if any; c) what aspects of active packaging should be considered by other legislative sectors, e.g. by those dealing with direct food additives, food authenticity and food labelling. To address these questions, the project had 6 objectives. 1. Define and evaluate the size of the present and likely future market for active packaging in the UK, the types of packaging involved, the active ingredient(s) and the types of food in contact. 2. Evaluate the migration potential for those applications identified 3. Make recommendations for further work, including any experimental work if required 4. Evaluate if standard migration test protocols are adequate for the applications identified

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5. Make a critical evaluation of the report from the European Project Actipak 6. Make recommendations within CEN TC194 if standard test protocols are found to be wanting.

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2. THE PRESENT MARKET FOR ACTIVE PACKAGING IN THE UK The types of packaging involved, the active ingredient(s) and the types of food in contact are considered here. A number of active packaging systems are used in the UK presently. These include: Traditional applications 2.1 Wooden barrels for whisky Wooden barrels are very widely used for the storage and maturation of whisky, wine and other alcoholic drinks and this has been practiced for a very long time. This packaging application has both releasing and absorbing character, to change and improve the organoleptic qualities of the stored spirit. To help do this, the barrels may be pre-treated by flaming to char the interior of the wood. The barrels may also be used first with e.g. sherry wine to incorporate flavour, aroma and colour components that may subsequently re-migrate into the spirit. Absorbers 2.2 Meat pads and fish pads In these applications, pads are used to absorb the drip from meat, poultry and fish in display packs. As such they fall under the category of an absorber of food-related chemicals, being moisture/humidity control agents. They are very widely used. Their construction is usually a laminate of plastic gauze, adhesive and cellulose fibre pad and the food contact surface is the plastic. Other absorbent pads may contain water-imbibing polyacrylamide granules. Scavengers 2.3 Plastic fruit bags with an ethylene scavenger incorporated These bags are occasionally advertised by mail-order companies. The plastic is polyethylene which is impregnated with a mineral such as powdered pumice stone. It is claimed that the mineral acts as an ethylene scavenger and as such this application falls under the category of an absorber of food-related chemicals. Ethylene itself is a hormone for fruit ripening and it is claimed that fruit placed in the active bags keep for longer in the home. With an inorganic mineral the ethylene is trapped on the active ingredient. Another mode of action is possible using permanganate absorbed onto silica gel to oxidise ethylene first to acetaldehyde and then to ethanol [12]. It is not clear from the literature if the oxidation products are trapped on the silica or if they are released into the internal pack atmosphere. Further oxidation, to form acetic acid, is also possible in principle because permanganate is a strong oxidising agent. Permanganate-containing sachets have not been found in use in the UK. The topic of ethylene scavengers has been reviewed [13].

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2.4 Oxygen scavengers Oxygen scavengers find limited use at present in the UK, in high-value meat packs (e.g. salami [12]) and in bottled beers. In these two applications, an absorber of oxygen is used to supplement the gas-barrier properties of the primary packaging material. The food is packaged in the absence of oxygen in the case of meat it is vacuum-packed or packed under nitrogen gas, whereas beers are packed under an atmosphere of carbon dioxide. The role of the oxygen absorber is then to scavenge any oxygen that may permeate through the primary packaging and which would otherwise spoil the flavour of the product. The chemicals used to react with oxygen include powdered iron [14], ascorbate and sodium sulfite. The chemical can be incorporated into the primary packaging (e.g. into the crown cap of a bottle or into the bottle wall [15]) or as a sachet insert [16]. These applications are not common. For example, the use of oxygen scavengers in high-value meat was estimated to be about 150 M units in the UK in 2001 [12]. Releasers 2.5 Fungicides used in fruit wrappers Biphenyl (E230) and orthophenyl phenol (E231 and its sodium form E232) are widely used as a post-harvest fungicide for citrus fruits imported into the UK [17]. They can be applied to the fruit surface directly using immersion baths or as a spray, individually or in combination with imazilil and/or thiabendazol. E231 and E230 are also used to impregnate fruit wrappers [18]. In this application, they act as fungistatics which migrate from the wrapping paper to the fruit to inhibit post-harvest microbial decay [19]. E 230, E 231 and E 232 were temporarily authorised under Directive 95/2/EC for treatment of citrus fruits. As these substances are to be considered as plant protection products, they fall under Directives 91/414/EEC and 90/642/EEC. For the sake of consistency, their withdrawal from Directive 95/2/EC has been proposed recently in a 5th amendment to Directive 95/2/EC on food additives other than colours and sweeteners [20]. 2.6 Microwave susceptors Microwave susceptors are materials used for crisping and browning foods in microwave ovens. Under the definitions of active packaging described in Section 1.1 they are modifiers of physical properties. Examples of their use include packaging for pizzas, chips and popcorn. Microwave susceptors in current use are bi- or tri- laminate in structure. Bi-laminate materials comprise a poly(ethylene terephthalate) (PET) film as the food contact surface which is coated with a thin film of aluminium. This is glued onto a paperboard backing. Tri-laminate materials also comprise metallised film with a paper backing but have an overlying layer of paper as the food contact surface. Microwave susceptors are not intentional releasing systems but the high temperature generated (ca. 200C or more) can give rise to thermal breakdown of their constituents and accelerated migration [21, 22, 23, 24].

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2.7 Antimicrobial substances used to protect/preserve the food contact material Examples include the use of silver releasers in plasticised PVC cling film food wrap [25] and Triclosan (2,4,4' -trichloro-2' -hydroxydiphenyl ether) [26] in a wide range of food contact materials and articles on sale to UK industry (e.g. conveyor belts and other food processing equipment) and consumers (e.g. kitchenware). Although these applications are often considered to be active packaging, strictly they are not because there is no intention to exert any preservative effect on the food. Exerting a preservative effect using Triclosan is still at the concept stage only [27, 28, 29]. Rather, the antimicrobial agent is incorporated into materials and articles with the declared function of releasing the substance to the surface only, thereby maintaining the hygienic properties and/or the cleanability of the plastic surface. Insofar as the active ingredients are not intended to migrate into the food and that any migration that does occur is incidental to the intended function, then these applications fall within the scope of the framework directive 89/109/EEC. However, it will be necessary to demonstrate that any incidental migration that there may be, does not act as a food preservative.

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3. THE LIKELY FUTURE MARKET FOR ACTIVE PACKAGING IN THE UK With the exception of wooden barrels for whisky and fruit wrapping papers, the UK applications listed above are all absorbing rather than releasing systems. Furthermore, the use of active packing with some exceptions is not at all widespread in the UK. By contrast, active packaging materials are both more numerous and are used much more widely in the USA and especially in Japan. This probably reflects the different legislative systems that operate. It has been noted [12] that many of the concepts and technologies for active packaging have been available for the past 20 years and yet they have not been commercialised significantly outside of Japan and South-East Asia. 3.1 Absorbing/Scavenging systems The major market in Japan and the USA is for oxygen scavengers. The applications include, amongst others, packaging pasta, milk powder, biscuits, beers, and cooked meats [30]. Sales of oxygen scavenging systems in Western Europe was estimated to be 10M units in 1998 and 300M units in 2001. Forecast sales [31] of oxygen scavenging systems in Western Europe in 2004 are 2,100M units, rising to 5,700M units in 2007. The next most important application is probably moisture absorbers/regulators. In the simplest form the moisture absorbers are pads with absorbent fibrous materials as described in Section 2.2.2 above and used in meat, poultry and fish packs. For more sophisticated moisture regulators, sachets of plastic films containing the active ingredient are used. The active ingredient can be hydroscopic materials such as concentrated sugar solutions, water-imbibing polyacrylamide, or silica gel. In other scavenging applications, enzymes are incorporated into the packaging material with the aim to remove lactose from milk and milk products or cholesterol from liquid egg and milk [32] or to remove bitter components from fruit juices [33, 34]. 3.2 Releasing systems The most significant difference between the UK (and Europe) and Japan/USA is in the commercial exploitation of releasing systems in the latter countries. A brief overview of these applications is of interest here because it indicates what may enter the European market place if proposals [11] to modify the EU Framework Directive are carried-through. Forecast sales [35] of antibacterial and preservative releasers in Europe, Japan and the USA in the year 2004 are 140 and 4 M respectively, rising to 207 and 22 M respectively in 2007. 3.2.1 Antimicrobial releasers A number of chemical release systems are designed to exert a preservative effect on the food via an antimicrobial activity. Antimicrobials [36, 37] for, typically, meat and bakery products. This includes formaldehyde [38], small organic acids (e.g. propionic [39], sorbic [40], benzoic [41] acids) and ethanol emitters (e.g. silicon dioxide
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impregnated with ethanol and contained within a paper/plastic laminate, releasing ethanol by displacement by water vapour absorbed from the food [42]). Sulfur dioxide released from metabisulphite, for cooked meats and meat products. Silver releasing systems. Chlorine dioxide released from (propriety) inorganic precursors. Carbon dioxide releasers (from water-absorption into a dry-mix of sodium hydrogen carbonate and ascorbate). Antimicrobials obtained from plant extracts [37] (e.g. methyl chavicol and linalool from basil, allyl isothiocyanate from horseradish/mustard [43]) or from other biobased sources (e.g. the bacteriocin nisin, a protein with activity against gram-negative bacteria which is an approved food additive in some countries [44, 45]) 3.2.2 Antioxidant releasers A number of chemical release systems are designed to exert a preservative effect on the food via an antioxidant activity. Bakery products such as biscuits and cereal products are target market applications. Butylated hydroxy anisole and butylated hydroxy toluene (BHA and BHT). Vitamin E (alpha-tocopherol, [46, 47]). Phenolics from plant extracts (e.g. from Oregano and Rosemary [48, 49]).

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These active packaging concepts can be appreciated more clearly by considering two case studies. CASE STUDY 1. A releasing system Allyl Isothiocyanate from horseradish / mustard Most early examples of active packaging both releasers and absorbers - have an add-on character to be used along with the primary packaging material. They take the form of sachet inserts or stick-on strips or labels placed in- or onto existing non-active food packages. A typical example is the use of allyl isothiocyanate, obtained from horseradish or mustard, as an antimicrobial substance. This application is advertised as being on sale in Japan [50]. Format 1. External label containing the active ingredient The active ingredient is incorporated into an external label that is attached to the outside of the primary packaging. The active ingredient permeates as a gas through the packaging film and treats the food surface. External label Food

In this format there are restrictions on the type of primary packaging films that can be used. Since the active ingredient must penetrate the primary packaging film, the film must not be impermeable. Polyethylene (20~100 m thick) and oriented polypropylene (10 to 20 m thick) are said to be suitable whereas oriented polystyrene, polyethyleneterephthalate and cellulose have insufficient permeability. On the other hand, an atmosphere of the active ingredient must be established within the packaging and so materials that are too permeable are not suitable either. These include paper, non-woven fabrics and plasticised PVC films. Format 2. Internal label containing the active ingredient If an internal label is deployed then impermeable packaging films can used. In this format, however, the label itself and any chemicals that may be used to contain or encapsulate the active ingredient to give a controlled release rate (e.g. allyl isothiocyanate held within a cyclic oligosacharide), may incidentally come into direct contact with the food. Internal label Food

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The internal label is functionally equivalent to sachet technology. It may simply be considered to be an immobilised sachet secured to the inside of the primary packaging material. Format 3. Internal film containing the active ingredient In this format, which is an extension of the internal label format, the active sheet is not laminated to the inside of the primary packaging but, rather, is placed inside the packaging on top of the food and can make either direct contact or incidental contact during transport etc. Sheet Food

CASE STUDY 2. A scavenging system A photo-initiated oxygen-scavenging plastic If early examples have an add-on character and take the form of sachet inserts or stick-on strips or labels placed in- or onto existing non-active food packages, then in more recent examples the active function is engineered into the primary packaging material from the outset. This appears to be the direction that the food industry wishes to take, with the active function incorporated into barrier technology rather than using sachet technology [12]. Despite the fact that sachet technology is used widely in Japan, European consumers do seem to be resistant to sachet technology. One reason may be the fear that the sachet could be mistaken by consumers to contain a seasoning to be applied to the food product [51]. The development of certain oxygen-scavenging plastic films came about from a chance observation. When nylon was laminated to PET, the residual cobalt from the polymerisation catalyst in certain grades of PET caused photo-initiated oxidation of the nylon with consequent scavenging of oxygen. The commercial exploitation of these laminates as, for example, plastic beer bottles, was not possible because the oxidation products formed from the nylon were poorly understood and were considered to have the potential to migrate into the bottled product giving an organoleptic problem. Nevertheless, this chance discovery gave the impetus to develop other oxygen-scavenging plastics. In one example, a proprietary oxidisable substrate is incorporated into the polymer backbone as a monomer. A uv-photoinitiator and an oxidation catalyst are formulated into the plastic as additives. The food is packaged in the film,
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which is then activated using a short burst of uv-light to start the scavenging of oxygen from the atmosphere that surrounds the food. Because the oxidisable substrate is polymer-bound then it is intended that the oxidation products are too, and so they will not migrate. Each part of the three-component system the monomer and the two additives are subject to the normal petition process to have monomers and additives placed on the positive list of substances used to make plastics intended for food contact in the EU [52]. One commercial product using this approach is the Cryovac OS2000 range of films which have an oxidisable co-polymer layer laminated to a PVDC outer layer which provides a barrier and so directs the oxygen-scavenging activity towards the pack interior [53, 54, 55, 56]. Although the oxygen-scavenging activity is triggered by irradiation using uv light, it has been reported that the films have a limited shelf-life of about three months on the reel [54].

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4. EVALUATE THE MIGRATION POTENTIAL FOR THE APPLICATIONS IDENTIFIED A large number of applications for active and intelligent packaging are at various stages of development or commercialisation. It is helpful to describe the different components of the systems in generic terms, to facilitate a systematic examination of their migration potential. As part of this project, CSL participated in a DG-SANCO task force of technical experts, to examine these issues in 2002 and 2003. The following definitions and descriptions emerged [57]. 4.1 Definitions active releasing materials and articles - deliberately release substances into the packaged food or the environment surrounding the food. active absorbing materials and articles - deliberately absorb substances from the packaged food or from the environment surrounding the food. active ingredients - components deliberately incorporated in an active material or article. carrier - means the material used to contain the active or intelligent ingredient For example: with an internal sachet or label, or an external label Primary packaging Carrier with the active ingredient Food

Or if the carrier for the active ingredient is the primary packaging material itself as a mono or bi/multi-layer: Primary packaging containing the active ingredient Food

4.2 Intentional transfer (release) of substances to the food This can be either through direct contact or indirectly through the package headspace gas.

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The active agent. The active ingredients clearly fall within the regulations on Direct Food Additives (since the addition is intentional and not incidental) and they would require specific authorisation as such. Special tests may be needed to verify efficacy under actual and foreseeable conditions of use. For example, if relying on chemical migration (a diffusion process) to supply the active ingredient to the food, it might be necessary to demonstrate that an effective concentration was in place in the food soon after packaging, that the concentration did not exceed any limit value towards the end of the shelf life, and that migration was not too high or too low at different temperatures during packaging, transport and storage. Precursors to the active agent (the active ingredient). The emphasis here is on substances that may incidentally migrate but are not intended to migrate in order to perform their function. These substances are then considered as packaging migrants and should be dealt with in the normal petitioning process [58] to gain approval. If restrictions are needed then they will be assigned a specific migration limit, as normal. The carrier. The carrier system for the active ingredient - e.g. a sachet insert or panel patch or the primary packaging impregnated - would need to comply with the normal rules for composition and migration of/from materials and articles intended to come into contact with foodstuffs. Migration test conditions may need to be tailored on a case-by-case basis because of the specialist conditions of use. 4.3 Intentional removal (scavenging) of substances from the food The active ingredient. Such applications do not currently fall within the scope of regulations on food contact materials since the framework directive 89/109/EEC deals with the transfer of constituents to foodstuffs. Products of the scavenged substance(s). In certain cases the scavenging activity is by a chemical reaction. Examples are the scavenging of ethylene by permanganate (to form ethanol, acetaldehyde and acetic acid), scavenging of oxygen by iron to form iron oxide, and the scavenging of oxygen by an oxidisable polymer to form polymer-bound products. The identity and potential migration of these intentional transformation products would need consideration. The carrier. The carrier system for the active ingredient would need to be evaluated as described above for releasing systems. 4.4 General observation on scavenging systems There are important aspects to be considered here by other legislative sectors. If the packaging maintains freshness e.g. by maintaining an inert atmosphere and the food does not age/degrade, then it could stretch the publics normal perception of what constitutes fresh. But insofar as the packaging is inert then this falls within the normal principles and procedures whereby packaging materials and articles are approved. However, if an active packaging maintains
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only the appearance of freshness, e.g. by scavenging undesirable degradation products [59], then this could be a problem. This is quite a philosophical as well as a technical question. Examples of spoilage indicators are short aldehydes formed as fats autoxidise and go rancid [60], and the low molecular weight amines evolved as fish suffers microbial attack [59]. If not dealt with properly, active packaging could give rise to quality problems where the food has aged but the consumer cannot tell. At worst, it could give rise to safety questions if the food may have spoiled with microbial growth but the consumer cannot detect this because the spoilage indicators are absent (scavenged). 4.5 General observations on active ingredients There are many substances used or likely to be used in active packaging that are not presently on any positive list or inventory list. Examples include the components in a gas scavenging system (e.g. permanganate for ethylene, iron powder for oxygen) or the exotic transition metals in thermochromic dyes used in time-temperature indicators. These components may be acceptable because there is no direct contact made with the food and this is achieved using a barrier layer to migration. However, in the absence of an agreed definition of a functional barrier, along with the necessary agreed definition of no-migration (e.g. limit of detection; threshold of regulation; threshold of toxicological concern) then the legislative status of these non-contact substances is unclear. This is not a unique situation, because similar questions apply to the components of printing inks, adhesives and secondary packaging all of which are not intended to touch the food directly. An accommodation for these non-contact substances used in active and intelligent packaging is needed. This must be provided by an assessment of their migration potential which by necessity would have to be application-specific (case-by-case) and not a generic assessment.

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5. EVALUATION OF THE ACTIPAKREPORT This large European project was funded under the 5th Framework programme. The project [9] had five key tasks: 1. An in-depth review of technologies, legislation, market and consumer needs and trends in active and intelligent packaging in relation to current European food packaging regulations. 2. A study of the analytical composition and migration behaviour of selected active and intelligent concepts: this will be used to determine a classification in view of the restrictions of current legislation. Combinations of food and packaging will be selected and prepared for testing. 3. An investigation of: 3.1 the safety of the selected concepts through microbial safety analysis 3.2 the risks from false indications 3.3 the effectiveness of the concept' sensory, microbial and chemical shelfs life extending capacity 3.4 the efficiency of the concepts as scavengers of, for example, oxygen, ethylene. 4. Examination of the toxicological properties of selected active and intelligent packaging concepts, 4.1 their economic and environmental effects 4.2 the attitude of European consumers to these innovative concepts. 5. Discussion with EU and national authorities about legislative aspects of active and intelligent packaging and drafting of amendments specific to these concepts. Modification of current migration testing methods and development of procedures for systematic evaluation of the fitness for food contact of active and intelligent concepts. With the review of the area described in chapters 1 to 4 in this report, it can be concluded that the Actipak project was successful in identifying and disseminating the main topics of interest here that is, those aspects that have a potential impact on consumers with respect to food quality and safety. The process and the outcome of the Actipak project contributed in part to the formulation of the principles discussed [57] for a draft regulation on active and intelligent packaging that encapsulates all the key points identified. a) should comply with the Framework Directive on FCMs b) should not mislead the consumer e.g. What does fresh mean? c) should be suitable and effective for the intended purpose of use e.g. verify efficacy ? d) comply with Directives 92/59/EEC (general product safety) and 87/357/EEC (misleading and unsafe claims) e.g. with scavenging of spoilage indicators (e.g. fish, meat) then food may have spoiled but the consumer cannot detect this. e) active absorbing or intelligent ingredient must be authorised e.g. establishment of a Community list submit data for its safety evaluation by EFSA
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f) intelligent ingredients not listed, may be used provided that they are separated from the food by a functional barrier. functional barrier needs definition g) Overall migration limit of 60 ppm however, the amount of the active releasing ingredients shall not be included in the determination of OM h) SMLs for authorised active absorbing and intelligent ingredients shall be established i) verification of compliance to be carried out in accordance with the (normal) rules however, if the tests cause physical or other changes which do not occur in use, other test conditions and/or food simulants may be used provided that they represent the worst conditions not causing these changes j) active ingredients (themselves or their by-products) which may become components of the food must comply with all the community provisions on food additives, flavourings etc this would apply with respect to types of foods, max levels, purity criteria etc

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6. APPLICABILITY OF EXISTING MIGRATION TEST PROTOCOLS Evaluate if standard migration test protocols are adequate for the applications identified Make recommendations within CEN TC194 if standard test protocols are found to be wanting.

6.1 The test procedures and simulants already available Migration test protocols are fairly well established for ceramics and plastics. For other types of materials, such as paper and board, rubber and elastomers, no harmonised test protocols exist. It is likely that most present and future active packaging applications will be based on plastics as the primary packaging and carrier materials. Plastics are controlled [61] by an overall migration limits (OML), specific migration limits (SML), compositional limits on a mass-fraction basis (QM) and compositional limits on a mass-area basis (QMA). The guiding principle in the EC Directives on plastics, is that migration testing should mimic the worst foreseeable conditions of actual use with food [62]. This includes taking into account the chemical and physical state of the packaged food, along with the nature and extent of the contact. The migration limits in the regulations apply to the foodstuffs themselves or, alternatively, to so-called food simulants. Simulants are selected to mimic the essential features of the different food categories. Type of food aqueous foods acidic foods alcoholic foods fatty foods dry foods Simulant distilled water acetic acid solution, 3% ethanol solution, 10% or higher olive oil, or alternative oils (no simulant specified)

There is extensive guidance available on the selection of appropriate conditions and test methods for overall migration and specific migration [63, 64]. It is likely, however, that if these protocols - simulants, time and temperature conditions of test - are applied to active and intelligent packaging materials without due regard to any special construction features or modes of application with foodstuffs, then misleading test results could be obtained. There is presently no simulant or test conditions specified for indirect contact (gas phase migration) or for contact with dry foods for which gas-phase migration could be important. Many of the active or intelligent systems rely on their active function (absorbing or releasing) operating through the gas phase. So testing for undesirable gas-phase migration should be considered.

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6.2 Applicability of existing migration test procedures 6.2.1 The physical nature of the food simulants commonly used The carrier of the active ingredient must be permeable to some extent, to allow the release or absorption of substances. In the case of pouch or sachet inserts, the exchange of substances is via the gas phase (e.g. oxygen, moisture, ethylene, off-odours) and the carrier is not intended to come into direct contact with the food. Rather, it simply resides in the atmosphere within the food package. Many of these carriers are permeable to liquid simulants and these simulants would cause a physical change that would not occur during normal conditions of use with the food. Consequently, alternative simulants may be required that are not liquids. Another example is meat pads used for moisture control. When first placed in contact with the meat or fish, there is a flux of liquid from the meat into the pad. However, if the pad approaches saturation, then there is the possibility of migration in the opposite direction, from the pad to the meat. This may bring components of the adhesive into contact with the food. It might be inappropriate to test such pads by total immersion or single-sided contact with a liquid food simulant, but some migration testing would be required for example into a semi-solid food simulant with liquid absorbed onto a carrier [65]. These situations are already foreseen in the Plastics sector, which states that if tests under the contact conditions specified cause physical or other changes in the test specimen which do not occur under worst foreseeable conditions of use of the material or article, then the worst possible conditions not causing these changes should be used. 6.2.2 The chemical nature of the food simulants commonly used In certain cases, the conventional simulants may be too aggressive chemically. An example would be if the active packaging were iron physically mixed into a polymer as an oxygen scavenger. This may give excessive migration if tested using 3% acetic acid whereas this might not occur in acidic foods. In these cases, an alternative simulant should be considered that more closely mimics the behaviour of the food. 6.2.3 The nature of the test apparatus employed In some applications, the carrier of the active ingredient may be too small to test using conventional single-sided test apparatus and so specialised migration cells may be required. A sandwich technique using conventional simulants and test conditions may be suitable these tests [66]. 6.3 Standardisation of new analytical methods If as envisaged [57, 67] the commission proposes a new specific measure on active and intelligent packaging along with case-by-case evaluation of migration potential, then CEN TC194 will need to respond to mandates from the commission for the development of new application-specific standard test protocols.

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Woodhead Publishing Ltd., Cambridge, UK and CRC Press, Boca Raton:USA, 2001. ISBN 1-85573-462-1. [63] EN1186. Part 1. Guide to the selection of conditions and test methods for overall migration. [64] EN13130. Part 1. Guide to the test methods for the specific migration of substances from plastics into food and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants. [65] K. Mountfort, J. Kelly, S. M. Jickells & L. Castle. A critical comparison of four test methods for determining overall and specific migration from microwave susceptor packaging. Journal of Food Protection, 1996, 59, 534-540. [66] R. Rijk. Active & intelligent packaging systems and the legislative aspects. Abstracts of lectures of the Actipak unwraps Europe conference on Active and intelligent packaging for food. Held in Amsterdam (NL), 20-21 January 2003, pp15-21. [67] Document EMB/973. Working document. Draft Commission Regulation on active and intelligent materials and articles intended to come into contact with foodstuffs (version updated to 27.10.2003).

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