Saturated and aromatic mineral oil hydrocarbons from paperboard food packaging: estimation of long-term migration from contents in the paperboard and data on boxes from the market

In the absence of a functional barrier, mineral oil hydrocarbons from printing inks and recycled fibres tend to migrate from paper-based food-packaging materials through the gas phase into dry food. Concentrations easily far exceed the limit derived from the acceptable daily intake (ADI) of the Joint FAO/WHO Expert Committee on Food Additives (JECFA). Since the estimation of long-term migration into the food by testing at 40°C for 10 days is difficult, it seems preferable (and easier) to use the mineral oil content in the paperboard. Evaporation experiments showed that hydrocarbons eluted up to about n-C₂₄ are sufficiently volatile for relevant migration into dry food: in worst-case situations, about 80% migrate into the packed food. The extraction of the paperboard was optimised to give good recovery of the relevant hydrocarbons, but to discriminate against those of high molecular mass which tend to disturb gas chromatographic analysis in on-line coupled normal phase HPLC-GC-FID. Even though some of the relevant hydrocarbons had already evaporated, the average concentration of?<?C₂₄ mineral oil saturated hydrocarbons (MOSH) in the paperboard boxes of 102 products from the Swiss and Italian market was 626?mg?kg^?1. Nearly 15% of investigated boxes still contained more than 1000?mg?kg^?1?<?C₂₄ MOSH up to over 3000?mg?kg^?1 (maximum?=?3500?mg?kg^?1). This amount of MOSH in the board have the potential of contaminating the packed food at a level exceeding the limit, derived from the JECFA ADI, hundreds of times.     

Migration of mineral oil from printed paperboard into dry foods: survey of the German market

From the German market, 119 samples of dry food were analyzed for the migration of mineral oil. The products selected were packed in paperboard boxes and intended for storage for extended periods of time at ambient temperature. The 0.6 mg/kg limit for mineral oil saturated hydrocarbons (MOSH) derived from the WHO/JECFA evaluation was frequently exceeded by a factor of 10–100. Typically, 10–20% of the migrating mineral oil consisted of aromatic hydrocarbons (MOAH). Most samples were merely 2–3 months old and far from the end of their shelf life (usually 1–3 years). From the assumption that about 70% of the MOSH and MOAH which are eluted from GC up to the C₂₄ n-alkane (<C24) end up in the food (potential of migration), it was estimated that migration might almost triple before the products reach the end of their shelf life, reaching 31 mg/kg on average, with several samples exceeding 100 mg/kg. At the time of the analysis, products without an internal bag and with a bag of paper or polyethylene reached up to about 80% of the potential of migration (average, 30–50%). Bags of polypropylene, acrylate-coated polypropylene, PET or with an aluminum layer seemed to block migration (with one possible exception), but it was premature to reach conclusions on long-term functional barrier properties. From the comparison with <C₂₄ MOSH concentrations in unprinted recycled paperboards, it was estimated than on average about a quarter of the migrating mineral oil was from printing ink used for decorating the box.     

Migration of mineral oil from printed paperboard into dry foods: survey of the German market. Part II: advancement of migration during storage

In April 2010, 119 samples of dry foods packed in paperboard boxes and stored at ambient temperature were collected from the German market. The migration of mineral oil from the recycled paperboard and printing ink was analyzed for the first time immediately after collection and reported in Vollmer et al. (Eur Food Res Technol 232:175–182, 2011). It frequently exceeded 10–100 times the 0.6 mg/kg limit for mineral oil saturated hydrocarbons (MOSH) derived from the WHO/JECFA evaluation published in 2002. As most samples were far from the end of the shelf life, analyses were repeated 4 months later and a third time either at the expiry date or after 16 months. The average MOSH concentration in the foods increased from 8.9 to 14.3 mg/kg (by 60 %), which indicates a rapid migration during the first months of storage, but also a further increase up to the end of the shelf life. The maximum migration reached 101 mg/kg. In the third measurement, the average concentration of the migrated mineral oil aromatic hydrocarbons was 2.2 mg/kg, with a maximum at 13.2 mg/kg. Most types of food behaved similarly, differences mostly reflecting the types of packaging rather than the food properties. Exceptions were table salt (hardly any migration) and noodles (low migration). Internal bags with an aluminum foil or PET layer were complete barriers. Migration through plastic with vapor-deposited aluminum or acrylate-coated polypropylene was reduced, but still sometimes exceeded 0.6 mg/kg. Internal bags of polyethylene had a weak effect on slowing migration, but acted as a sink for mineral oil: Although on average they only constituted 1.1 % of the total mass of the packs, they absorbed nearly 40 % of the migrating hydrocarbons. Polypropylene was a similar sink. In addition, it strongly slowed migration, but at the third measurement the 0.6 mg/kg limit was nevertheless exceeded in 11 of 16 samples. Polyolefin oligomeric saturated hydrocarbons (POSH) from the plastic or heat-sealable layer, largely branched hydrocarbons similar to MOSH, often migrated in the range of 1–5 mg/kg.     

Migration kinetics of mineral oil hydrocarbons from recycled paperboard to dry food: monitoring of two real cases

Mineral oil hydrocarbons present in printing inks and recycled paper migrate from paper-based food packaging to foods primarily through the gas phase. Migration from two commercial products packed in recycled paperboard, i.e. muesli and egg pasta, was monitored up to the end of their shelf life (1 year) to study the influence of time, storage conditions, food packaging structure and temperature. Mineral oil saturated and aromatic hydrocarbons (MOSH and MOAH, respectively), and diisopropyl naphthalenes (DIPN) were monitored using online HPLC-GC/FID. Storage conditions were: free standing, shelved, and packed in transport boxes of corrugated board, to represent domestic, supermarket and warehouse storage, respectively. Migration to food whose packs were kept in transport boxes was the highest, especially after prolonged storage, followed by shelved and free-standing packs. Tested temperatures were representative of refrigeration, room temperature, storage in summer months and accelerated migration testing. Migration was strongly influenced by temperature: for egg pasta directly packed in paperboard, around 30 mg kg^?1 of MOSH migrated in 8 months at 20°C, but in only 1week at 40°C. Muesli was contained into an internal polyethylene bag, which firstly adsorbed hydrocarbons and later released them partly towards the food. Differently, the external polypropylene bag, containing pasta and recycled paper tray, strongly limited the migration towards the atmosphere and gave rise to the highest level of food contamination. Tests at increased temperatures not only accelerated migration, but also widened the migration of hydrocarbons to higher molecular masses, highlighting thus a difficult interpretation of data from accelerated simulation.     

The analysis of saturated and aromatic mineral oil hydrocarbons in dry foods and from recycled paperboard packages by online HPLC–GC–FID

ABSTRACT

The purpose of this study was to determine the concentrations of mineral oil hydrocarbons in dry foodstuffs packed in recycled paperboard, which were imported from different foreign countries to Germany. After collection, mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in dry foodstuffs and recycled paperboard were analysed using online coupled high-performance liquid chromatography–gas chromatography–flame ionisation detection (online HPLC–GC–FID) far before the end of the shelf life of the samples. Our results showed that recycled paperboard has MOAH content higher than that of dry foodstuffs. The proportion of MOAH within total mineral oil hydrocarbons was determined to be 7–45% in dry foodstuffs and 4–48% in paperboard. In addition, 29% of the products were found to contain over 1.00 mg/kg MOAH, with a maximum of 2.72 mg/kg in oatmeal. White colour recycled paperboard contained lower amounts of MOSH and MOAH than that of brown and grey colour recycled paperboard. The MOSH concentration in dry foodstuffs ranged from 0.11 to 21.92 mg/kg (?C25 hydrocarbons), which may be an indication of rapid migration. The lowest determined MOSH concentrations (?C25 hydrocarbons) were found in sea salt and soda samples, even when their paperboard contained high mineral oil hydrocarbons. Our three samples in packages containing internal bags (for complete barriers) were found to have low mineral oil concentration due to reduced migration through plastic (acrylate-coated polypropylene). However, one sample, a ‘crispy’ product with an internal bag, contained the extreme amount of 21.92 mg/kg. Differences in contaminants observed in both dry foodstuffs and recycled paperboard may have been due to the different packaging and production techniques of the different countries. In addition, 8 of 24 dry foodstuff samples contained MOSH concentrations frequently exceeding the 2.0 mg/kg limit for MOSH C₂₀–C₃₅.     

Migration of mineral oil,photoinitiators and plasticisers from recycled paperboard into dry foods: a study under controlled conditions

Migration from recycled paperboard was monitored after 2, 4 and 9 months of storage for six test foods industrially packed in five configurations, four with internal plastic films. After 9 months, the migration of mineral oil saturated hydrocarbons into foods directly packed in the paperboard amounted to 30–52 mg/kg, which corresponded to 65%–80% of those of a volatility up to that of the n-alkane C₂₄ in the paperboard. The concentration of the migrated aromatic hydrocarbons in the foods ranged from 5.5 to 9.4 mg/kg. More than half of this migration occurred in the first 2 months. Differences between the foods amounted to mostly less than a factor of 2 and seemed to be related to porosity or permeability more than fat content. Nine photoinitiators were detected in the paperboard, of which eight migrated into the packed food at up to 24%. Several plasticisers were present in the recycled paperboard, but only butyl phthalates showed significant migration. After 9 months, up to 40% of diisobutyl phthalate and 20% of dibutyl phthalate migrated into the food with direct contact. The internal polyethylene film hardly slowed migration, but the film and the tray absorbed approximately three times more mineral oil than the food, despite constituting merely 4% of the mass of the pack. Oriented polypropylene strongly slowed migration: The highest migration of saturated hydrocarbons measured after 9 months (2.3 mg/kg) corresponded to only 3% of the content in the paperboard and included migrated polyolefin oligomeric saturated hydrocarbons. Coating of polypropylene with an acrylate further slowed the migration, but the migration from the paperboard was still detectable in four of the six samples. Polyethylene terephthalate was a tight barrier.     

Enrichment for reducing the detection limits for the analysis of mineral oil in fatty foods

A German draft for a regulation requires that there must be no migration of mineral oil aromatic hydrocarbons (MOAH) from recycled paperboard into food. The Federal Institute for Risk Assessment (BfR) is requested to establish the detection limit. It was previously shown that the detection limit of the commonly used methods is below 0.1 mg/kg for the majority of the foods, but substantially higher in fatty products because of limited capacity of the liquid chromatographic preseparation to retain fat, interference by olefins and, if also the mineral oil saturated hydrocarbons (MOSH) should be analyzed, the natural paraffins primarily consisting of odd-numbered n-alkanes. A method is described for the enrichment of the MOSH and MOAH conceived as an auxiliary tool for fatty foods analyzed by the conventional methods, such as on-line HPLC–GC. In a double bed liquid chromatographic column, the lower packing consists of a mixture of activated aluminum oxide, silica gel with silver nitrate and activated silica gel, the upper of activated silica gel. The technical detection limit in edible oils is below 0.3 mg/kg, which translates to less than 0.1 mg/kg in the dry foods packed in recycled paperboard. The distinction between migrated mineral oil and that present before packaging often presupposes the availability of the food prior to packaging.     

Activated carbon added to recycled paperboard to prevent migration into food: approach for determining efficacy,and first results

Catcherboard MB12® from Smurfit Kappa is a recycled paperboard incorporating activated carbon to reduce the release of contaminants into food. An approach is proposed to determine the efficacy of the activated carbon. Sorption into activated carbon increases the concentration ratio paperboard/food (distribution coefficient) and reduces the migration rate, i.e. prolongs the time for equilibration. Using silicone paper as food simulant, the concentration ratio was increased by a factor of at least 1000 compared to recycled paperboard without activated carbon, which is sufficient to meet the 1% criterion proposed for barriers. Sorbents have limited capacity. A load with in total 4000 mg surrogate substances/kg paperboard (in addition to the material from the paperboard) exceeded the capacity: concentration ratios were reduced and the release of paperboard constituents increased. Capacity is consumed by constituents from the printing inks and the packed food. Total amounts of substances in dry foods of sufficient volatility to potentially migrate into the paperboard through the gas phase at ambient temperature were determined by GC-FID. For the large majority of the dry foods, these amounts were clearly below the capacity limit even under the exaggerated assumption of total transfer. Migration of mineral oil hydrocarbons into cat food over up to 1 year was not detectable at 1 mg/kg. It is concluded that recycled paperboard with activated carbon is promising for respecting the 1% criterion stipulated for functional barriers to avoid food contamination from recycled paperboard.     

Migration of selected hydrocarbon contaminants into dry semolina and egg pasta packed in direct contact with virgin paperboard and polypropylene film

Migration of mineral oil saturated hydrocarbons (MOSH), polyolefin oligomeric saturated hydrocarbons (POSH), and polyalphaolefins (PAO from hot melts) into dry semolina and egg pasta packed in direct contact with virgin paperboard or polypropylene (PP) flexible film was studied. Migration was monitored during shelf life (up to 24 months), through storage in a real supermarket (packs kept on shelves), conditions preventing exchange with the surrounding environment (packs wrapped in aluminium foil), and storage in a warehouse (packs inside of the transport box of corrugated board). Semolina pasta packed in virgin paperboard (without hot melts) had a MOSH content lower than 1.0 mg kg^?1. An increasing contamination with PAO belonging to the adhesives used to close the boxes was detected in egg pasta, wrapped in aluminium (1.5 and 5 mg kg^?1 after 3 and 24 months, respectively). An environmental contribution to total hydrocarbon contamination was observed in egg pasta kept on shelves that, after 3 and 24 months, showed levels of PAO/MOSH < C₂₅ around 3 and 10 mg kg^?1, respectively. The migration of POSH from PP film into egg pasta wrapped in aluminium was around 0.6 mg kg^?1 after 3 months of contact and reached 1.7 mg kg^?1 after 24 months of contact. After 9 months of contact, semolina pasta packed in PP film and stored in the transport box showed that some MOSH migrated into the pasta from the board of the transport box (through the plastic film).     

Potential for short-term migration of mineral oil hydrocarbons from coated and uncoated food contact paper and board into a fatty food simulant

ABSTRACT

Mineral oil hydrocarbons (MOH) are widely used in the food industry for applications such as printing inks, additives, adhesives, and processing aids for food additives. Recently, the migration of MOH from food contact paper and board into foods has raised public health concerns. In this study, a total of 110 food contact paper and board samples, including baking and cooking paper (23), baking cups (28), food packaging bags (22), lunch boxes (8), party plates (26), and straws (3) were evaluated to quantify the content and short-term migration levels of MOH. The MOH were separated into mineral oil saturated hydrocarbons (MOSH)/polyolefin oligomeric saturated hydrocarbons (POSH) and mineral oil aromatic hydrocarbons (MOAH) via a validated on-line liquid chromatography?gas chromatography?flame ionisation detection (LC–GC–FID) technique. The coating materials of the sample products comprised polyethylene, polypropylene, polyethylene terephthalate, and silicone. The effects of the coating materials on the content and migration of MOH/POSH were evaluated. Quantitative analysis of the MOH in the samples showed that the MOSH/POSH and MOAH content varied widely, ranging from 16 to 5626 mg kg^?1 for MOH, regardless of the coating materials. Short-term migration of MOSH/POSH was observed only in samples with polyolefinic coatings, such as polyethylene and polypropylene, in experiments conducted at 25 °C for 10 min, although the extent of MOAH migration for all samples was at the trace level. The migration of MOSH/POSH was detected within the range of 0.93 to 62.3 μg L^?1 in 22 samples, and the migration of MOAH was detected within the range of 0.80 to 2.6 μg L^?1 in only 4 samples. These results demonstrate that although the short-term migration potential of MOH is generally negligible, the migration of MOSH/POSH into wet fatty foods can be accelerated by polyolefinic coatings, even within a very short time.     

快餐包装纸中矿物油向固体食品模拟物的迁移

研究从市场上收集到的24 种快餐包装纸中的矿物油向固体食品模拟物Tenax的迁移规律。在多个不同的迁移条件（40 ℃/0.5、1、2、3 h,40 ℃/10 d和70 ℃/2 h）,探究矿物油的迁移行为及其影响因素,以评价其安全性。选择正己烷-乙醇（1∶1,V/V）混合溶液对Tenax进行过夜萃取,采用质量分数0.3%硝酸银固相萃取柱对饱和烃矿物油（mineral oil saturated hydrocarbons,MOSH）和芳香烃矿物油（mineral oil aromatic hydrocarbons,MOAH）进行分离纯化,最后用气相色谱-氢火焰离子化检测法和气相色谱-质谱法分别进行定量和定性分析。结果表明：随着温度的升高,多种快餐包装纸中矿物油向Tenax的迁移量也随之增加。涂蜡纸中MOSH迁移量均有所检出,其数值为110.49～615.40 mg/kg,而MOAH部分均未检出,这可能是因为涂蜡纸表面涂覆的石蜡层属于MOSH类,导致其MOSH部分的迁移量较高。网购餐盘纸和常规餐盘纸中MOSH迁移量约为其特定限量值（0.6 mg/kg）的10～400 倍,MOAH的迁移量约为其特定限量值（0.5 mg/kg）的10～70 倍,而使用优质胶印油墨的原生纤维餐盘纸均未超过其限量值。最后,通过对印有胶印油墨的原生纤维餐盘纸中矿物油进行溯源分析,发现经过迁移的矿物油一部分可能来源于其所用油墨,其他来源可能来自于回收纤维、黏合剂、添加剂和加工助剂等。     

Migration of mineral oil from party plates of recycled paperboard into foods: 1. Is recycled paperboard fit for the purpose? 2. Adequate testing procedure

Party plates made of recycled paperboard with a polyolefin film on the food contact surface (more often polypropylene than polyethylene) were tested for migration of mineral oil into various foods applying reasonable worst case conditions. The worst case was identified as a slice of fried meat placed onto the plate while hot and allowed to cool for 1?h. As it caused the acceptable daily intake (ADI) specified by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) to be exceeded, it is concluded that recycled paperboard is generally acceptable for party plates only when separated from the food by a functional barrier. Migration data obtained with oil as simulant at 70°C was compared to the migration into foods. A contact time of 30?min was found to reasonably cover the worst case determined in food.     

Is recycled newspaper suitable for food contact materials? Technical grade mineral oils from printing inks

Recycled paper and board used in food packaging materials (boxes, paper bags) often cause migration of mineral oil into food at levels which are unacceptable according to present toxicological assessments. When foods in recycled board are densely packed into larger boxes or onto pallets, most of the hydrocarbons up to n-C₂₀ may migrate into the packed food within a few weeks, those up to n-C₂₈ at a decreasing rate. Unprinted recycled board contained 300–1,000 mg/kg mineral oil <n-C₂₈. The main sources are the inks used for printing newspapers: newspapers contained roughly 3,000 mg/kg mineral oil <n-C₂₈. These mineral oils fall into classes for which JECFA established a tolerable daily intake of 0.01 mg/kg body weight. Using standard assumptions for calculating specific migration limits, a maximum tolerable concentration in food of 0.6 mg/kg is derived. This evaluation assumes highly refined white oils, whereas the oils found in recycled board are of technical quality and contain 15–25% aromatic compounds, predominantly with 1–3 aromatic rings, as shown by comprehensive GC × GC. This finding precipitates authorities into a dilemma: recycling is supported for the sustainable use of materials, but on the basis of present toxicological assessments the migration is often far beyond acceptable.     

Migration of mineral oil from party plates of recycled paperboard into foods: 1. Is recycled paperboard fit for the purpose? 2. Adequate testing procedure

Party plates made of recycled paperboard with a polyolefin film on the food contact surface (more often polypropylene than polyethylene) were tested for migration of mineral oil into various foods applying reasonable worst case conditions. The worst case was identified as a slice of fried meat placed onto the plate while hot and allowed to cool for 1 h. As it caused the acceptable daily intake (ADI) specified by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) to be exceeded, it is concluded that recycled paperboard is generally acceptable for party plates only when separated from the food by a functional barrier. Migration data obtained with oil as simulant at 70°C was compared to the migration into foods. A contact time of 30 min was found to reasonably cover the worst case determined in food.     

Migration of bisphenol A and benzophenones from paper and paperboard products used in contact with food

Migration of bisphenol A (BPA) and benzophenones, i.e., benzophenone (BZ), 4-(dimethylamino)benzophenone (DMAB), Michler's ketone (MK) and 4,4'-bis(diethylamino)benzophenone (DEAB), from 21 paper and paperboard products (15 recycled paperboard boxes and 6 virgin paper products) used in contact with food was examined. Migration levels of compounds from recycled paperboard were compared under various food-simulating conditions. BPA showed the highest migration into 20% ethanol and benzophenones into 95% ethanol. No compounds migrated from virgin paper products, but compounds did migrate into food simulants from recycled paperboard food boxes. BPA migrated into 20% ethanol from all recycled paperboard food boxes between 1.0 and 18.7 ng/mL. Into 95% ethanol, migration of BZ was observed in 8 samples (1.0-18.9 ng/mL), DMAB in 12 samples (1.2-3.7 ng/mL), MK in 13 samples (1.9-9.0 ng/mL), and DEAB in 13 samples (1.0-10.6 ng/mL). The highest migration level was 27.2 ng/mL and most of the migration levels were below 10 ng/mL. These values are sufficiently low compared with the TDI and NOAEL levels. Moreover, the amount of food in daily meals that comes into contact with paperboard products is relatively small. Consequently, it was concluded that there was no safety concern regarding the tested compounds in recycled paperboard food boxes.     

Update on recycled paperboard and its compliance for food contact

The last 3 years brought much movement around the migration from recycled paperboard in general and of mineral oil in particular. It has been shown that it is unrealistic to ensure the safety of the many and variable migrants from recycled fibers. The toxicological evaluation of mineral oil remains uncertain, but the strong accumulation of certain saturated mineral hydrocarbons in human tissues might increase the concern. The draft of a German regulation on mineral oil migration from recycled paper and board struggles with the difficult analysis in food, but frequent measurement in food is avoidable if the compliance work can be based on citable systematic studies. In the discussions about potential solutions, the introduction of barriers prevails. Internal bags with barrier layers have been widely introduced. For packings without internal bags, barriers on the internal surface of the recycled paperboard have been developed, but not yet introduced into the market on broad scale. An agreed method for measuring barrier efficiency and a specification of minimum required efficiency are probably a prerequisite. Work for an industry standard on barriers is on-going in Switzerland.     

纸质食品包装材料的矿物油迁移研究进展

食品中的矿物油污染物是指石油来源的C10~C50烃类化合物, 包括烷烃矿物油(mineral oil saturated hydrocarbons, MOSH)和芳烃矿物油(mineral oil aromatic hydrocarbons, MOAH)2大类。近年来的研究表明, 食品中的矿物油污染物主要来源于食品的回收纸包装材料迁移。本文综述了国外近十年来纸质包装材料的矿物油迁移研究情况, 包括纸质包装材料迁移的矿物油分析方法——液相色谱-气相色谱联用法; 矿物油迁移至食品的2种方式: 气态扩散迁移和包装材料接触迁移; 降低矿物油迁移的技术方法, 即食品包装纸质材料的回收工艺, 向包装纸质中添加活性炭等吸附剂以及增加阻隔层以阻挡矿物油的迁移。旨在为相关企业和机构提供数据与技术参考。     

Analysis of mineral oil in food: results of a Belgian market survey

ABSTRACT

Recently, migration of mineral oil components from food contact materials into various foods has been reported. The analysis of mineral oil in food is complicated since it consists of mineral oil saturated hydrocarbons (MOSH) comprising a complex mixture of linear, branched and cyclic compounds and variable amounts of mineral oil aromatic hydrocarbons (MOAH), mainly alkylated. Both MOSH and MOAH form ‘humps’ of unresolved peaks in the chromatograms with the same range of volatility. Since these two fractions have a different toxicological relevance, it is important to quantify them separately. Occurrence data on mineral oil are available only for a limited number of food groups and only from few countries. In Belgium, data on the contamination of food by mineral oil are lacking. In this contribution, an in-house validated online combination of liquid chromatography with gas chromatography (LC–GC) with flame ionisation detection (FID) was used for the quantification of MOSH and MOAH. Totally, 217 packed food samples were selected using a well-defined sampling strategy that targeted food categories which are highly consumed and categories suspected to contain mineral oil. For 19 samples, the method was not applicable. For the 198 remaining samples, MOSH was detected in 142 samples with concentrations up to 84.82 mg kg^?1. For the MOAH fraction, there are 175 samples with a concentration below the limits of quantification (LOQ), while 23 samples had a higher concentration ranging from 0.6 to 2.24 mg kg^?1. Finally, these results were compared with the action thresholds as proposed by the Scientific Committee (SciCom) of the Belgian Food Safety Agency (FAVV-AFSCA). Only one sample exceeded the threshold for MOSH, while the threshold for MOAH was exceeded in 23 samples. For the samples exceeding the action threshold, further investigation is needed to identify the contamination source.     

Comparability of mineral oil testing for dry food and cardboard samples – Perspectives from different PT rounds

Mineral oil hydrocarbons (MOH) can be found in detectable levels in a multitude of foodstuffs. Therefore, chemical analysis of food for MOH gains importance. Different proficiency testing (PT) rounds on mineral oil testing have been performed in different matrices: cereals and rice as well as cardboard samples were examined. The laboratories participating in the PT rounds had to follow specific requirements for examination. The sample materials used contained different concentrations of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH). The PT results were statistically evaluated according to ISO 13528:2005 and additionally the HorRat(R) value was calculated to gain information on the comparability of the mineral oil testing. It could be shown that for the examined sample materials and under the chosen specifications for testing a comparable determination of the mineral oil content is possible within the required relative standard deviations. A useful analytical determination can be achieved with an acceptable relative standard deviation of <50% from a concentration of defined mineral oil fractions at ≥1 mg/kg in food. In the concentration range for MOH in food of between 1 mg/kg and 2 mg/kg, relative standard deviations of 20–40% were achieved. MOH concentrations of ≥ 2 mg/kg food were determined with good relative standard deviations of around 20%. Moreover, due to the results gained within this work a statement concerning the comparability for MOSH and MOAH contents below concentrations of 1 mg/kg food is possible: under the chosen conditions for examination as part of this work, mineral oil determination below 1 mg/kg food showed high variability. To gain reliable information with regard to consumer protection on the risk of mineral oil contents in this low concentration range further standardisation of the test method is indicated.     

Effectiveness of polypropylene film as a barrier to migration from recycled paperboard packaging to fatty and high-moisture food.

The capability of a polypropylene (PP) film barrier to prevent migration of residual contaminants from recycled paperboard into food simulants was studied. Anthracene, benzophenone, methyl stearate and pentachlorophenol were chosen as chemical surrogates to represent classes of contaminants likely to be found in recycled paper/paperboard. Each surrogate was spiked into a test specimen made of seven thin virgin paper layers at concentrations of 1-50 mg kg(-1). Test specimen were dried, stacked and sandwiched with PP films, laminated with PP film and then subjected to migration experiments using a compression cell maintained at 100 degrees C for 2 h. The concentration of the surrogates in the test specimen and in 95% ethanol, isopropanol and 10% ethanol food-simulating solvents was determined by gas chromatography with flame ionization and electron capture detection. The results show that although the concentrations of the surrogates in the food simulants decreased with an increase in PP film thickness, they were still high and generally resulted in dietary concentrations >0.5 microg kg(-1), the level that US Food and Drug Administration would equate with negligible risk for a contaminant migrating from food packaging. Only at the lowest spiking level (1 mg kg(-1) benzophenone) did migration from the paperboard through a 0.127-mm PP film result in a dietary concentration of 相似文献