Australian survey of acrylamide in carbohydrate-based foods

A method was developed and validated for the determination of acrylamide in carbohydrate-based foods. Solid-phase extraction employing a mixed-bed anion and cation exchange cartridge in series with a C18 extraction disk was used to clean-up water extracts of food samples before analysis by liquid chromatography coupled with tandem mass spectrometry detection. The limit of detection was calculated as approximately 25 μg kg^-1 and the limit of reporting was 50 μg kg^-1. The average method recovery for 84 samples from a range of matrices reporting was 99% with a relative standard deviation of 11.2%. A survey was conducted of 112 samples of carbohydrate-based foods composited from 547 products available in the Australian market. The analytical results were used in conjunction with Australian food consumption data derived from the 1995 National Nutrition Survey (NNS) to prepare preliminary dietary exposure estimates of Australians to acrylamide through only the food groups examined. Mean dietary exposure to acrylamide resulting from consumption of the foods tested, for Australians aged 2 years and above, was estimated as 22-29 µg day^-1 (equivalent to 0.4-0.5 µg kg^-1 bodyweight day^-1) and between 73 and 80 µg day^-1 (1.4 and 1.5 µg kg^-1 bodyweight day^-1) for 95th percentile consumers. Young children (2-6 years) consuming acrylamide-containing foods had a higher acrylamide exposure on a per kilogram bodyweight basis (mean 1.0-1.3 µg kg^-1 bodyweight day^-1). The estimated exposure of Australians to acrylamide is similar to that estimated for other countries.     

Migration and sensory properties of plastics-based nets used as food-contacting materials under ambient and high temperature heating conditions

Overall migration from a wide range of commercial plastics-based netting materials destined to be used as either meat or vegetable packaging materials into the fatty food simulant isooctane or the aqueous simulant distilled water, respectively, was studied. In addition, sensory tests of representative netting materials were carried out in bottled water in order to investigate possible development of off-odour/taste and discoloration in this food simulant as a result of migration from the netting material. Sensory tests were supplemented by determination of the volatile compounds' profile in table water exposed to the netting materials using SPME-GC/MS. Test conditions for packaging material/food simulant contact and method of overall migration analysis were according to European Union Directives 90/128 (EEC, 1990) and 2002/72 (EEC, 2002). The results showed that for both PET and polyethylene-based netting materials, overall migration values into distilled water ranged between 11.5 and 48.5 mg l^-1, well below the upper limit (60 mg l^-1) for overall migration values from plastics-packaging materials set by the European Union. The overall migration values from netting materials into isooctane ranged between 38.0 and 624.0 mg l^-1, both below and above the European Union upper limit for migration. Sensory tests involving contact of representative samples with table water under refluxing (100°C/4 h) conditions showed a number of the netting materials produced both off-odour and/or taste as well as discoloration of the food simulant rendering such materials unfit for the packaging of foodstuffs in applications involving heating at elevated temperatures. GC/MS analysis showed the presence of numerous volatile compounds being produced after netting materials/water contact under refluxing conditions. Although it is extremely difficult to establish a clear correlation between sensory off-odour development and GC/MS volatile compounds' profile, it may be postulated that plastics oxidation products such as hexanal, heptanal, octanal and 2,6 di-tert-butylquinone may contribute to off-odour development using commercially bottled table water as a food simulant. Likewise, compounds such as carbon disulfide, [1,1'-biphenyl]-2-ol and propanoic acid, 2 methyl 1-(1,1-dimethyl)-2-methyl-1,3-propanediyl ester probably originating from cotton and rubber components of netting materials may also contribute to off-odour/taste development.     

Sorption of aroma compounds in PET and PVC during the storage of a strawberry syrup

The sorption of 14 aroma compounds into PET and PVC was monitored during storage of a strawberry syrup for 1 year. Concentrations in the syrup and in the polymer were determined during storage and compared with previously published results obtained with glass bottles. Apparent partition coefficients between the polymer and the syrup (noted K_app) were estimated from experimental kinetics without reaching equilibrium K_app values and optimally identified from the kinetic data obtained between 30 and 90 days. They exhibited a similar behaviour for both polymers with values were between 2 × 10^-5 and 2 × 10^-3, 4 × 10^-5 and 3 × 10^-2, respectively, for PET and PVC. The variation of K_app values in PET was mainly correlated to the polarity of tested compounds as assessed by their log P values. By contrast, the variations in K_app values for PVC were mainly related to their chain lengths. Due to slightly higher partition coefficients and diffusion coefficients in PVC compared with PET, the amount of absorbed aroma was four times higher in PVC than in PET; however, the amount of absorbed aroma compounds was less than 0.1% of the initial amount present into the syrup, except for octyl butanoate. The variation in concentration in the syrup was interpreted as a combination of a degradation process and a transport process into the packaging material. Both effects were particularly noticeable for both PET and unstable aroma compounds.     

Migration of 2-butoxyethyl acetate from polycarbonate infant feeding bottles

An enforcement campaign was carried out to assess the migration of 2-butoxyethyl acetate (2-BEA) from polycarbonate infant feeding bottles intended for repeated use. Migration was measured by three successive migration tests into two of the European Union official food simulants: distilled water and 3% acetic acid testing at 40°C for 10 days. The Danish Veterinary and Food Administration (DVFA) has assessed that a migration above 0.33 mg for 2-BEA and a group of eight related substances kg^-1 foodstuff from plastics articles used exclusively for infants is unacceptable. Migration of 2-BEA was found from eight of 12 bottles. However, migration above the target value of 0.33 mg kg^-1 was not observed in the third decisive test from any of the 12 different brands of polycarbonate feeding bottles. A migration of between 0.05 and 0.26 mg kg^-1 from seven of 12 bottles was measured to 3% acetic acid in the third test, whereas no migration to distilled water was observed in the third test. The average recovery of 2-BEA after the 10-day exposure at the target value of 0.33 mg kg^-1 was 77% into distilled water and 36% into 3% acetic acid. The limited recovery was understandable as 2-BEA was partly hydrolysed in the aqueous food simulants and 2-butoxyethanol, a hydrolysis product and one of the related substances was identified. Quantification was carried out using gas chromatography after liquid/liquid extraction of the food simulant.     

Exposure to antimony from polyethylene terephthalate (PET) trays used in ready-to-eat meals

Antimony residues, a result of the use of a polycondensation catalyst in the production of polyethylene terephthalate (PET) oven-proof trays, were analysed in ready-to-eat meals. The toxicity of antimony has raised concerns about consumer safety; therefore, the migration of small fractions of these residues into ready meals and foods as a result of cooking directly in the PET trays was studied. A straightforward approach of measuring real samples was selected to obtain accurate exposure data. Background antimony concentration was determined separately from a series of lunch meals, which ranged from not detectable to 3.4 µg kg^-1. Microwave and conventional oven-cooking caused a distinct increase in the concentration of antimony in food and ready meals of 0-17 and 8-38 µg kg^-1, respectively, depending, to a certain extent, on the industrial preparations. The migrated quantities of antimony corresponded to 3-13 µg. For comparison, PET roasting bags and ready-made dough products in PET baking dishes were also evaluated. About half of the products prepared at a temperature of 180°C exceeded the specific migration limit set for food contact material by the European Commission. However, the migrated amounts of antimony relative to the accepted tolerable daily intake (TDI) show that exposure from this type of food is currently not of toxicological concern.     

Survey of formaldehyde, acetaldehyde and oligomers in polyethylene terephthalate food-packaging materials

Polyethylene terephthalate (PET) is frequently used as a packaging material for beverage bottles, fruit and vegetable trays, and egg crates in Japan. Levels of formaldehyde (FA), acetaldehyde (AA) and PET oligomers in various PET food packaging were determined. PET samples were initially dissolved in trifluoroacetic acid with 2,4-dinitrophenylhydrazine to derivatize formaldehyde and acetaldehyde to their dinitrophenylhydrazones. The stable derivatives along with the oligomers were analysed using HPLC with ultraviolet light detection at 360 and 254 nm, respectively. The PET pellets contained 3.5-12.4 µg g^-1 AA and 4.0-7.2 mg g^-1 oligomers, while FA was below the determination limit. FA, AA and oligomer levels in Japanese bottles were 0.6-3.0 µg g^-1, 8.4-25.7 µg g^-1 and 5.0-8.7 mg g^-1, ND-1.6 µg g^-1, 5.0-13.1 µg g^-1 and 4.9-8.2 mg g^-1 in French and Italian bottles, and ND-1.2 µg g^-1, 9.1-18.7 µg g^-1 and 5.6-8.0 mg g^-1 in US and Canadian bottles, respectively. Compared with European bottles, Japanese bottles contain higher FA and AA levels. In sheet-moulding products, their contents were determined as ND-1.1 µg g^-1, 11.5-43.1 µg g^-1 and 4.6-9.2 mg g^-1, respectively. The results show that sheet-moulding products contain lower FA and higher AA in comparison with bottles. FA and AA are considered to be generated from PET during the heating process for moulding the pellets to bottles or sheet-moulding articles and de-aeration during the sheet-moulding process is effective in removing FA. In contrast, the level of the oligomers remains unchanged during the moulding process from pellets to bottles or sheet products.     

Migration of aniline from polyamide cooking utensils into food simulants

Migration of aniline from polyamide cooking utensils was investigated. Aniline was found to originate from the application of black colorant in the polyamide 66 raw material. Analysis of polyamide raw material revealed an aniline concentration of 121 ± 13 mg kg^-1. The aniline concentration in a cooking utensil (turner) manufactured with 70% polyamide raw material was 82 ± 6 mg kg^-1. When testing migration from black coloured samples of turner, whisk and cooking spoon into water simulant at 100°C for 30 min, the migration levels at the third exposure were 39 ± 1, 11 ± 4 and 37 ± 4 μg dm^-2, respectively. Hence, these articles were not compliant with respect to the area-based limit for primary aromatic amines (3.33 μg dm^-2) set by European Union Directive 2002/72/EC. Repeated testing of a cooking utensil (turner) showed that approximately 100 h use at 100°C was required to reach legal (non-detectable) levels of aromatic amine migration.     

Consumer exposure to substances in plastic packaging. I. Assessment of the contribution of styrene from yogurt pots

A generic methodology for the assessment of consumer exposure to substances migrating from packaging materials into foodstuffs during storage is presented. Consumer exposure at the level of individual households is derived from the probabilistic modeling of the contamination of all packed food product units (e.g. yogurt pot, milk bottle, etc.) consumed by a given household over 1 year. Exposure of a given population is estimated by gathering the exposure distributions of individual households to suitable weights (conveniently, household sizes). Calculations are made by combining (i) an efficient resolution of migration models and (ii) a methodology utilizing different sources of uncertainty and variability. The full procedure was applied to the assessment of consumer exposure to styrene from yogurt pots based on yearly purchase data of more than 5400 households in France (about 2 million yogurt pots) and an initial concentration c₀ of styrene in yogurt pot walls, which is assumed to be normally distributed with an average value of 500 mg kg^-1 and a standard deviation of 150 mg kg^-1. Results are discussed regarding both sensitivity of the migration model to boundary conditions and household practices. By assuming a partition coefficient of 1 and a Biot number of 100, the estimated median household exposure to styrene ranged between 1 and 35 µg day^-1 person^-1 (5th and 95th percentiles) with a likely value of 12 µg day^-1 person^-1 (50th percentile). It was found that exposure does not vary independently with the average consumption rate and contact times. Thus, falsely assuming a uniform contact time equal to the sell-by-date for all yogurts overestimates significantly the daily exposure (5th and 95th percentiles of 2 and 110 µg day^-1 person^-1, respectively) since high consumers showed quicker turnover of stock.     

Migration of trimellitic acid from epoxy anhydride can coatings into foods

The migration of trimellitic acid and its esters from epoxy anhydride coatings was determined in simulants as well as in canned foods. The most appropriate simulant was a combination of EC simulants B and C: 2% acetic acid/10% ethanol in water. The average migration into food was 900 μg kg^-1. This far exceeds the 50 μg kg^-1 for which the safety of trimellitic acid and its anhydride is ensured and the Swiss legal limit (QM(T) of 5 mg kg^-1 coating). Furthermore, much trimellitic acid migrated as (unidentified) esters, i.e. toxicological testing of free trimellitic acid is inadequate for the material that in reality migrates.     

Intake of ochratoxin A and deoxynivalenol through beer consumption in Belgium

Estimations of ochratoxin A (OTA) and 4-deoxynivalenol (DON) exposure of the Belgian population through beer consumption were made using the results of the recent Belgian food survey and the compiled data set of OTA and DON levels in conventionally and organically produced beers in 2003-05. For the consumers of organic beers, the daily intake of OTA was 0.86 (in 2003), 1.76 (in 2004) and 0.72 (in 2005) ng kg^-1 body weight (bw), considering the mean beer consumption (0.638 litres) and the average level of OTA in 2003, 2004 and 2005, respectively. Using the 97.5th percentile of beer consumption (1.972 litres), the corresponding OTA daily intakes were 2.65, 5.44 and 2.24 ng kg^-1 bw, which are close or above the tolerable daily intake (TDI) of 5 ng kg^-1 bw. For the consumers of conventional beers, the OTA intakes were low: 0.23, 0.23 and 0.11 ng kg^-1 bw day^-1 for the average beer consumption, in 2003, 2004 and 2005 against 0.72, 0.73 and 0.34 ng kg^-1 bw day^-1 when the 97.5th percentile level was considered. As for the DON intake, the estimates were quite low for both conventional and organic beer consumers when the provisional maximum TDI (PMTDI) of 1 µg kg^-1 bw was considered. Average consumption of organic beer led to daily intakes of 0.05 and 0.04 µg DON kg^-1 bw in 2003 and 2004, respectively, whilst for conventional beer, daily intakes were 0.07 and 0.05 µg DON kg^-1 bw. At the 97.5th percentile level of beer consumption, daily intakes of 0.15 and 0.13 µg kg^-1 bw were obtained for organic beers against 0.23 and 0.17 µg kg^-1 bw for conventional ones. The results showed that beer could be an important contributor to OTA exposure in Belgium, even though a declining trend seems to be apparent during the last year of monitoring. Therefore, efforts should be devoted to maintain the OTA levels as low as reasonably achievable, especially for organic beer.     

Flow-through spectrophotometric sensor for the determination of saccharin in low-calorie products

A simple, rapid and inexpensive monoparameter flow-through sensor has been developed for the determination of saccharin in low calorie and dietary products. The method is based on the transient adsorption of the sweetener on Sephadex G-25 solid phase packed to a height of 20 mm in the flow cell. The optimal transient retention of the synthetic sweetener, in terms of sensitivity and sampling frequency, was obtained when pH 2.75 citric acid-sodium citrate buffer 5 × 10^-3 M was used as a carrier at a flow-rate of 1.5 ml min^-1. Saccharin was determined measuring its intrinsic absorbance at 217 nm at its residence time. Calibration graphs for peak height and peak area were linear over the range 5.0-200.0 μg ml^-1, RSD 1.18%, and 1.0-200.0 μg ml^-1, RSD 0.78%, respectively. Saccharin was determined in several food samples measuring height or area peak, obtaining recoveries ranging between 98-104 and 99-102% for height and area peak, respectively. The procedure was validated for use in the determination of saccharin in low calorie and dietary products giving reproducible and accurate results.     

2-Isopropylthioxanthone (2-ITX) in food and food packaging materials on the German market

To elucidate the occurrence of the photo-initiator, 2-isopropylthioxanthone (2-ITX), more than 100 food products on the German market, packed in cartons, plastic cups and foils, were investigated. For this, a rapid method to detect 2-ITX in food packaging materials was established. In case of positive findings, the accompanying foodstuffs were analysed in a subsequent step using different extraction methods, depending on the fat content of the food. Determination of the photo-initiator was done by high-performance liquid chromatography with diode array and fluorescence detection (HPLC-DAD/FLD). Recoveries ranged between 94 and 106% for non-fatty (RSD ≤ 1.1) and between 80 and 105% for fatty foods (RSD ≤ 8.5). The limit of detection and limit of quantification were determined to 2 and 5 µg l^-1. 2-ITX was detected in 36 of 137 packages (26%) and significant migration occurred in 75% of the packaging materials tested positive. The levels of 2-ITX ranged up to 357 µg kg^-1 in orange juice.     

Clostridium perfringens and its toxins in minced meat from Kars, Turkey

The aim of this study was to determine the prevalence of Clostridium perfringens and its toxins in minced meat. A total of 96 minced meat samples were collected from local markets (16) and small butcher's shops (80) in Kars (Turkey). Samples were analysed for the presence of C. perfringens and its toxins using a commercially available ELISA kit. A total of 31 (32%) Clostridium spp. strains were isolated and 17 (55%) of these isolates were identified as C. perfringens. Four (25%) of the samples from local markets and 27 (34%) from small butcher's shops were contaminated with Clostridium spp. Furthermore, C. perfringens was isolated from two (12%) and 15 (19%) samples from local markets and small butcher's shops, respectively. Mean counts of Clostridium spp. were 2.2 ± 0.83 × 10² CFU g^-1 for local markets and 4.35 ± 8.53 × 10² CFU g^-1 for small butcher's shops; mean counts for C. porringers were 2.75 ± 0.21 × 10² and 6.82 ± 10.96 × 10² CFU g^-1 from markets and butcher's shops, respectively. The number of samples contaminated with both Clostridium spp. and C. perfringens was higher in small butcher's shops than in local markets. Moreover, higher numbers of Clostridium spp. and C. perfringens were isolated in samples from small butcher's shops than from local markets. A total of 13 (13%) samples were also positive for toxins produced by the organism, as detected by ELISA. Eleven samples from small butcher's shops and two samples from local markets were positive for the C. perfringens toxins tested. Moreover, two (12%), one (1%), four (4%) and two (2%) samples were contaminated with C. perfringens types A, B, C and D, respectively. In conclusion, some meat samples collected from local markets and small butcher's shops contained C. perfringens and its toxins and, therefore, present a potential risk of food poisoning.     

Annual variation of deoxynivalenol in Danish wheat flour 1998-2003 and estimated daily intake by the Danish population

The occurrence of deoxynivalenol (DON) in Danish wheat flour was studied during the period 1998-2003 by either capillary gas chromatography with electron capture detection and liquid chromatography coupled to an ion trap mass spectrophotometer. A total of 151 samples were collected from mills and the retail market in Denmark. Contamination levels varied considerably from year-to-year with the highest concentrations occurring in samples from the 2002 harvest with mean and median concentrations of 255 and 300 µg kg^-1, respectively. Compared to other harvest years, 2002 had the highest amount of precipitation around flowering time, i.e. from the end of June to the beginning of July covering weeks 25-27. The lowest average levels were found in samples from the 2001 harvest, where weeks 25-27 were dry compared with other harvest years. The highest value (705 µg kg^-1) was obtained in a flour sample from the 2002 harvest, but none of the tested samples exceeded the maximum limit of 750 µg kg^-1, which has been recently introduced by the European Commission for DON in flour used as raw materials in food products. Calculation of chronic or usual intake by a deterministic approach showed that intake did not exceed the TDI of 1 µg kg^-1 bw day^-1 either for the whole population or for children. A probabilistic approach also showed that intake in general was below the TDI, but intake for children in the 99% percentile amounted to more than 75% of the TDI. The highest intake is calculated to be 2.5 µg kg^-1 bw day^-1.     

Survey of the migration of melamine and formaldehyde from melamine food contact articles available on the UK market

The migration of melamine and formaldehyde, monomers used in the production of melamine-ware food contact articles, has been determined from 50 retail articles purchased in the UK. The food simulant 3% aqueous acetic acid was used as this is the most aggressive simulant towards melamine plastics. The test conditions used were repeated exposure to the simulant for 2 hours at 70°C, since the articles were all intended for general use including contact with hot foods and beverages. Melamine migrated from 43 of the 50 samples tested and formaldehyde migrated from all 50 samples. Directive 2002/72/EC specifies migration limits for both of these monomers in foods and food simulants. Melamine is restricted by a specific migration limit (SML) of 30 mg/kg (equivalent to 5 mg/dm²) and formaldehyde, along with hexamethylenetetramine expressed as formaldehyde, is restricted by a total (T) SML(T) of 15 mg/kg (equivalent to 2.5 mg/dm²). In all cases the migration of melamine was much lower than the SML for this monomer. The migration of formaldehyde exceeded the SML(T) for 5 of the 50 samples tested. The failure to comply with the SML(T) was accompanied by a number of visible surface effects including discolouration and/or pitting of the simulant contact surface and cracking of the articles. Similar surface effects were observed when one of the samples was exposed to fruit juice which confirmed the suitability of the exposure conditions and 3% acetic acid as a simulant for the articles tested. The ratio of specific migration to overall migration was consistent with, but did not prove, the hypothesis that high formaldehyde migration could be due to the use of excessive hexamethylenetetramine in the polymer formulation. All illegal products were voluntarily removed from the market by the product suppliers.     

Justifying the need to prescribe limits for toxic metal contaminants in food-grade silver foils

The use of silver foils in various food preparations is a common practice in Middle Eastern and South East Asian countries. The FAO/WHO Joint Expert Committee on Food Additives (JECFA) has included silver in the list of food additives, but specifications were not prepared. Indian food legislation has included food-grade silver foil and laid down a purity requirement of 99.9%. This leaves an unspecified margin of 0.1% or 1000 µg g^-1 for contaminants. Therefore, a study to investigate the levels of metallic contaminants in food-grade silver foil was undertaken. Of 178 foils analysed, 161 (90%) contained silver, whilst 10% were fraudulently made up of aluminium. In the case of silver foils, 46% of the samples adhered to the desired purity requirement of 99.9%, while 54% had a lower silver content. Copper was present in 86.3% of the silver foils, while chromium, nickel and lead contamination was found in over 54% of samples. Cadmium levels were detected in 28% of the silver foils and manganese was present in 6.8% of samples. In silver foils showing metal contaminants, average levels were found for nickel (487 µg g^-1), lead (301 µg g^-1), copper (324 µg g^-1), chromium (83 µg g^-1), cadmium (97 µg g^-1) and manganese (43 µg g^-1), which being appreciable justify the need to prescribe limits for some metals in food-grade silver foil as well as for silver powder used in confectioneries and medicinal preparations. The work reported here should encourage manufacturers to use high-purity raw materials and take suitable precautions to reduce unwarranted exposure of consumers to toxic metal contaminants.     

Migration of bisphenol A from can coatings—effects of damage, storage conditions and heating

Bisphenol A (BPA) is an important monomer used in the manufacture of epoxy resins for internal food can linings. Experiments were conducted to investigate the effects of different storage conditions and can damage on the migration of BPA to foods. These experiments were conducted in a systematic fashion by filling empty epoxyphenolic coated cans with four foods: soup, minced beef, evaporated milk and carrots and a food simulant (10% ethanol). Filled cans of each food type or simulant were then sealed and processed using appropriate conditions, before storage at three different temperatures: 5°C, 20°C and 40°C. For each of the storage regimes, 50% of the cans were dented to establish if this would lead to increased BPA migration. Cans were removed from these stocks at intervals of 1, 3 and 9 months storage at 5°C and 20°C or 10 days, 1 and 3 months at 40°C. Some initial problems of heterogeneity between samples was overcome by determining the amount of BPA in food as well as in the can lining. It was found that 80-100% of the total BPA present in the coating had migrated to foods directly after can processing by pilot plant filling with food or simulant, sealing and sterilization. This level was not changed by extended storage (up to 9 months) or can damage, indicating most migration was occurring during the can processing step. There was no noticeable difference, in this respect, between the different foods or the food simulant. Analysis of control samples (foods fortified with ∼0.1 mg kg^-1 BPA and contained in Schott bottles) showed that BPA was stable under both processing and storage. Experiments were also conducted to investigate the potential effects, on the migration of BPA from can coatings, of cooking or heating foods in the can prior to consumption. Food cans were purchased and the food either cooked or heated in the can. BPA was analysed prior to and after the heating/cooking process. It was concluded from the results that there were no appreciable differences in the BPA level before and after cooking or heating.     

Estimated intake of intense sweeteners from non-alcoholic beverages in Denmark

In 1999, 116 samples of non-alcoholic beverages were analysed for the intense sweeteners cyclamate, acesulfame-K, aspartame and saccharin. High contents of cyclamate close to the maximum permitted level in 1999 of 400 mg l^-1 were found in many soft drinks. The estimated intake of the sweeteners was calculated using the Danish Dietary Survey based on 3098 persons aged 1-80 years. The estimated intake with 90th percentiles of 0.7, 4.0 and 0.2 mg kg^-1 body weight (bw) day^-1 for acesulfame-K, aspartame and saccharin, respectively, was much lower than the acceptable daily intake (ADI) values of 15, 40 and 2.5 mg kg^-1 bw day^-1 for acesulfame-K, aspartame and saccharin, respectively. However, the 90th percentile of the estimated cyclamate intake in 1-3 year olds was close to the ADI value of 7 mg kg^-1 bw day^-1; and the 99th percentile in the 1-10 year olds far exceeded the ADI value. Boys aged 7-10 years had a significantly higher estimated intake of cyclamate than girls. The 90th percentile for the whole population was 1.8 mg kg^-1 bw day^-1. After the reduction in the maximum permitted level in the European Union in 2004 from 400 to 250 mg cyclamate l^-1, the exposure in Denmark can also be expected to be reduced. A new investigation in 2007 should demonstrate whether the problem with high cyclamate intake is now solved.     

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.