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Methods and approaches used by FDA to evaluate the safety of food packaging materials.

In the Federal Register of July 17 1995 (60 FR 36582), the US Food and Drug Administration (FDA) established a 'threshold of regulation' process. This process was established for determining when the extent of migration to food is so trivial that safety concerns would be negligible. The process exempts materials in food-contact articles whose use results in dietary concentrations at or below 0.5 ppb (microgram/kg) from the food additive listing regulation requirement. Carcinogens or substances that may be carcinogens are excluded from this regulation. This paper explores some of the ramifications of the threshold of regulation policy with respect to traditional migration testing. It examines the use of the threshold approach and migration modelling to estimate food additive exposures. These results indicate that modelling may be a reasonable alternative to traditional migration testing.

Animals↗

Migration studies from paper and board food packaging materials. 1. Compositional analysis.

A survey of 32 paper and board materials intended for food contact has been undertaken. Sample composition was analysed to identify chemicals with a potential to migrate to foods. Representative materials covering a range of uses such as aqueous and fatty foods, and use at ambient and elevated temperatures, were obtained from industry. The samples were examined in their unfinished state, even where the final form would have included lamination to plastics, printing, or other treatments. A comprehensive and systematic analytical approach was applied which included determination of volatiles by headspace GC-MS, extraction using water, ethanol and chloroform with subsequent analysis by GC-MS and HPLC, and multi-element screening by ICP-MS. The solvent extracts were also weighed to determine the total amount of material available for migration. A large number of volatile substances were identified with alkyl and aryl aldehydes predominating in the majority of samples. Substances identified in solvent extracts included 2,6-di-tert-butyl-4-hydroxytoluene (BHT), di-tert-butylphenol, benzophenone, 4,4'-bis(dimethyl amino) benzophenone (Michler's ketone), triphenyl methane, bicyclohexylphenylphenanthrene carboxylic acid (and its methyl ester) and abietic acid. Levels of these substances were however generally below 1 mg/kg paper. Of the inorganic elements, arsenic and mercury were not detected above the limits of determination of 1.8 and 0.4 mg/kg respectively in any of the 10 samples examined. Cadmium was detected in teabag tissue and in unbleached Kraft paper at 0.3 mg/kg. Chromium was present in seven samples at 1.1-7.8 mg/kg, whilst lead was present in nine of the 10 samples at levels ranging from 0.3 to 5.9 mg/kg.

Benzophenones↗

Antioxidants in food packaging: a risk factor?

It is current practice to test all new additives for packaging polymers for toxicity before permitting them to be used in food contact applications. However, many antioxidants and stabilizers act sacrificially and are converted to oxidation products in the process of preventing polymer degradation. In most cases, little is known about the toxicity of antioxidant transformation products, and in some cases there is reason to suspect that they may be more toxic than the chemicals from which they are derived. Two possible solutions are presently showing promise. The first is to chemically react the antioxidant or stabilizer with the polymer, either at the polymer synthesis stage or preferably during processing, so that neither the antioxidant nor its transformation products can be leached into food. The second is to use a biological antioxidant (e.g. alpha-tocopherol) whose oxidation chemistry and toxicology are known.

Antioxidants↗

Requirements for food packaged in polymeric films.

The requirements of barrier properties of packaging materials against environmental factors vary with food products. The chemical, physical, and biological mechanisms of food deterioration due to environmental factors, vital properties required in packaging materials, and developments in progress and future trends to maintain the required standard of food quality have been critically reviewed. Theoretical and experimental results for a variety of food products in relation to the properties of the packaging materials are discussed. Methods of prediction of food stability and their industrial applications are also emphasized by specific examples.

Cellophane↗

Antimicrobial properties of basil and its possible application in food packaging.

Basil (Ocimum basilicum L.) is a popular culinary herb, and its essential oils have been used extensively for many years in food products, perfumery, and dental and oral products. Basil essential oils and their principal constituents were found to exhibit antimicrobial activity against a wide range of Gram-negative and Gram-positive bacteria, yeast, and mold. The present paper reviews primarily the topic of basil essential oils with regards to their chemical composition, their effect on microorganisms, the test methods for antimicrobial activity determination, and their possible future use in food preservation or as the active (antimicrobial), slow release, component of an active package.

Anti-Bacterial Agents↗

[Hygienic properties of cellophane film intended for food packaging].

The cellophane films intended for wrapping food products were studied. Investigations have established the presence of these films of the cellulose xanthogenate and products of its decomposition, of carbon bisulphide in particular. With their joint presence the determination of carbon bisulphide and hydrogen sulphide was done colourimetrically, the sensitivity of this method being 0.005 mg/l. Migration of carbon bisulphide from the cellophane into the atmosphere and water was investivaged. An interconnection between the amount of the migrated carbon bisulphide and the odour of aqueous cellophane extracts was disclosed. To improve sanitary and chemical properties of cellophane a more intensive washing off of sulphur-containing compounds from it is recommended.

Carbon Disulfide↗

Chemical analysis and genotoxicological safety assessment of paper and paperboard used for food packaging.

This study presents the research on the chemical analysis and genotoxicity of 28 virgin/recycled paper products in food-contact use. In the chemical analysis, paper products were extracted by reflux with ethanol, and analyzed by gas chromatography/mass spectrometry. 4,4'-bis(dimethylamino)benzophenone (Michler's ketone: MK), 4,4'-bis(diethylamino)benzophenone (DEAB), 4-(dimethylamino)benzophenone (DMAB) and bisphenol A (BPA) were found characteristically in recycled products. Seventy-five percent of the recycled paper products contained MK (1.7-12 microg/g), 67% contained DEAB (0.64-10 micro g/g), 33% contained DMAB (0.68-0.9 microg/g) and 67% contained BPA (0.19-26 microg/g). Although, BPA was also detected in virgin paper products, the detection levels in the recycled products were ten or more times higher than those in the virgin products. The genotoxicity of paper and paperboard extracts and compounds found in them were investigated by Rec-assay and comet assay. Of the 28 products tested by Rec-assay using Bacillus subtilis, 13 possessed DNA-damaging activity. More recycled than virgin products (75% against 25%) exhibited such activity, which, of the compounds, was observed in BPA, 1,2-benzisothiazoline-3-one (BIT), 2-(thiocyanomethylthio)benzothiazole, 2,4,5,6-tetrachloro-isophthalonitrile, 2,4,6-trichlorophenol (TCP), and pentachlorophenol. The critical toxicant in one virgin paper product was concluded to be BIT. Eight samples with DNA-damaging activity were also tested by comet assay using HL-60 cells; six induced comet cells significantly (five times or higher than the control) without a decrease of viable cells. TCP, BZ, DEAB, and BIT also caused a slight increase in comet cells. In conclusion, we showed that most recycled paper products contain chemicals such as MK, DEAB, DMAB, and BPA, and possess genotoxicity. However, the levels of the chemicals in the recycled products could not explain their genotoxic effects.

Apoptosis↗

Cytotoxicological safety assessment of papers and boards used for food packaging.

Because of the lack of information about the possible transfer of toxic compounds from papers and boards to food, the overall cytotoxicity induced by six papers and 15 boards was investigated from water extracts prepared according to the European prestandard. Cytotoxicity measurements were based on RNA synthesis rate of human HeLa S3 cells. The tested virgin and recycled papers and boards were differentiated and classified according to their cytotoxicological quality, which ranged from absence of any cytotoxic effect to severe inhibition of RNA synthesis rate. The cytotoxicity level also varied according to the total amount of compounds detected by gas chromatography. No correlation was found between cytotoxicity and endotoxins contained in the samples. No significant difference in cytotoxicity was observed between the papers and boards produced from virgin fibres and from recycled fibres. Moreover, the products obtained from chemical pulp showed lower cytotoxicity than the products based on mechanical pulp. More generally, the cytotoxicological approach is promising for monitoring paper/board treatment-induced problems. Further work is required to assess a modified standard procedure for the preparation of water extracts specifically adapted to paper/board.

Chromatography, Gas↗

Alternative fatty food simulants and diffusion kinetics of nylon 12 food packaging.

The migration of laurolactam and cyclic di- and trimer of nylon 12 was assessed using three different films and five food simulants (olive oil, isooctane, 95% ethanol, 50% ethanol, water). Substitute test conditions for migration into olive oil according to European Union Directive EC/97/48 were applied using 95% ethanol and isooctane. Results showed that 95% ethanol overestimated while isooctane underestimated the respective migration into olive oil. Water was the best olive oil substitute, as migration of laurolactam into water and olive oil using the same temperature gave similar results. Additionally, diffusion kinetics of laurolactam were investigated by migration kinetic studies using isooctane and olive oil. Diffusion coefficients determined with isooctane were significantly higher than those found using olive oil. It was proved that isooctane had an interaction and olive oil was inert to the polymer. The diffusion conductance parameter, A(p), for nylon 12 determined using olive oil ranged from 0.3 to 0.6.

Dietary Fats↗

Injector-internal thermal desorption from edible oils. Part 2: chromatographic optimization for the analysis of migrants from food packaging material.

Injector-internal thermal desorption from edible oil or fat is a convenient sample preparation technique for the analysis of solutes in lipids or extracts from fatty foods. The injector temperature is selected to vaporize the solutes of interest while minimizing evaporation of the bulk material of the oil. This technique has been in routine use for pesticides for some time. Now its potential is explored for migrants from food contact materials, such as packaging, into simulant D (olive oil) or fatty/oily food, which means extending the range of application towards less volatile compounds. The performance for high boiling components was investigated for diisodecyl phthalate (DIDP) and diundecyl phthalate (DUP). Since the injector temperature needs to be as high as 260degreesC, some bulk material of the oil enters the column and must be removed after every analysis. This is achieved by a coated precolumn backflushed towards the end of each analysis. Desorption of the solutes is particularly efficient in the initial phase, when a thin sample film is spread on the liner wall, and is largely determined by the diffusion speed in the oil after the latter has contracted to droplets. An increased carrier gas flow rate during the splitless period supports the transfer into the column. It is concluded that the technique is attractive for migrant analysis, with DUP being at the upper limit of the boiling point.

Chromatography↗

Method of test and survey of caprolactam migration into foods packaged in nylon-6.

An analytical method for the determination of the nylon-6 monomer caprolactam in foods is described. The foodstuff was extracted with ethanol: water (1:2) containing capryllactam as internal standard and the extract was defatted using hexane. The extract was analysed by liquid chromatography coupled with mass spectrometry. The test method was calibrated down to 0.7 mg kg(-1). The repeatability of the method was good, with a relative standard deviation of 9% at the 15 mg kg(-1) level. The method was demonstrated to be accurate in an independent external check sample exercise. The new method was applied to the analysis of 50 retail foodstuffs packaged in nylon-6. Caprolactam was detected and confirmed in nine of the 50 food samples, in the range 2.8-13 mg kg(-1). The presence of caprolactam was indicated in a further 15 samples, in the range 0.8-11 mg kg(-1), but these samples did not meet all of the five confirmation criteria applied. All migration levels (both confirmed and unconfirmed) were below the European specific migration limit for caprolactam, which is 15 mg kg(-1). The average migration for all 50 samples, setting non-detectables at half the limit of detection, was 2.6 mg kg(-1) with a standard deviation of 3.1 mg kg(-1) (n = 50). All samples found to contain detectable levels of caprolactam migration were for applications involving heating the food in the packaging. They were packs of, for example, sausage meat for which the food would have been heat processed in the nylon casing, or they were nylon pouches for heating foods by boiling, microwaving or roasting.

Caprolactam↗

Enforcement of food packaging legislation.

A survey of the results of the analysis of samples of packaging materials, obtained from the Dutch market during the last 5 years is presented. The diethylether extracts of food contact polymers were analysed by GC-MS according to the Dutch testing system. Lists of the identified constituents in the extracts of polystyrene (PS), polypropylene (PP), polyethylene (PE), polyethylene terephthlate (PET) and polyvinylchloride (PVC) are given. More than 50 constituents were identified in the more than 1000 samples investigated. An estimation of the quantities of the extracted constituents has been made. In PVC the following compounds were present in relatively large quantities (10 times the height of the internal standards): diethylhexyladipate, dinonylphthalate, and other phthalates. However 68% of the extracts contained no peaks higher than the internal standards.

Food Packaging↗

A nondestructive leak detection method for flexible food packages using hydrogen as a tracer gas.

A nondestructive leak detection method developed at Technical Research Centre of Finland (VTT) was tested for both gas-flushed and vacuum flexible packages. In the method, a gas package containing 0.5 to 5.0% (vol/vol) hydrogen in nitrogen was positioned in a test chamber, a controlled vacuum was pulled in the chamber through a pipe connected to a hydrogen sensor, and leaking packages were detected by the sensor as increased H2 concentration. The H2 tracer gas (0.5 to 5.0%) was introduced into leaking finished vacuum packages at 200 kPa pressure. Within 1 to 4 s the developed test method was able to detect leaks down to 10 to 15 microns and 20 to 30 microns in diameter in commercially manufactured gas-flushed packages filled with roasted meat balls and vacuum packages filled with ground coffee, respectively. Before leak testing, the vacuum packages were charged with H2 for 30 s. The sensitivity and leak detection time of the test method were improved when the H2 concentration in the package was increased and when the free space in the test chamber was decreased. The evaluated H2 concentrations did not affect the sensory or microbiological quality of the roasted meat balls. This study clearly demonstrated that the hydrogen tracer gas leak detection method has potential to be further developed as a fast, nondestructive, on-line leak testing apparatus for flexible packages with or without a headspace.

Animals↗

Properties of polyethylene films with incorporated benzoic anhydride and/or ethyl and propyl esters of 4-hydroxybenzoic acid and their suitability for food packaging.

Benzoic anhydride and ethyl and propyl esters of 4-hydroxybenzoic acid (ETP and PRP, respectively, also termed parabens) incorporated into low density polyethylene (LDPE) film were studied with regard to migration into food and food simulants at 6 degrees C and 25 degrees C, and changes in selected properties of the film were investigated. Antimicrobials were incorporated into polymer film in concentrations of 5 g/kg and 10 g/kg. The addition of parabens into the polymer was more difficult than benzoic anhydride due to their volatility. For benzoic anhydride, 30-40% and 10-20% of the added amount was found to leach from the film into aqueous and olive oil food simulants, respectively. The migration into both water and olive oil followed a very similar course in the case of parabens. Migration levels over 90% and in the range of 70% to 80%, relative to the amount of agent in the film, were determined for ETP and PRP respectively. The incorporation of antimicrobials into the film significantly changed the functional characteristics of the packaging material, i.e. permeability of oxygen, carbon dioxide and water vapour, tensile strength, coefficient of friction, sealing strength and transparency. Shelf life tests with packaged cheese and toasted bread demonstrated the efficiency of the film containing 10 g/kg of BA against mould growth on the food surface during storage at 6 degrees C.

Anhydrides↗