Koni Grob

Aromatic Hydrocarbons of Mineral Oil Origin in Foods: Method for Determining the Total Concentration and First Results

An online normal phase high-performance liquid chromatography (HPLC)-gas chromatography (GC)-flame ionization detection (FID) method was developed for the determination of the total concentration of the aromatic hydrocarbons of mineral oil origin with up to at least five rings in edible oils and other foods. For some samples, the olefins in the food matrix were epoxidized to increase their polarity and remove them from the fraction of the aromatic hydrocarbons. This reaction was carefully optimized, because also some aromatics tend to react. To reach a detection limit of around 1 mg kg(-1) in edible oils, an off-line enrichment was introduced. Some foods contained elevated concentrations of white paraffin oils (free of aromatics), but the majority of the mineral oils detected in foods were of technical grade with 20-30% aromatic hydrocarbons. Many foods contained mineral aromatic hydrocarbons in excess of 1 mg kg(-1).

Food Contamination with Organic Materials in Perspective: Packaging Materials as the Largest and Least Controlled Source? A View Focusing on the European Situation

The comparison of the various sources of food contamination with organic chemicals suggests that in the public, but also among experts, the perception of risk is often distorted. Firstly, neither pesticides nor environmental pollutants contribute the most; the amount of material migrating from food packaging into food may well be 100 times higher. Secondly, control of these large migrants is often lagging behind the standards set up for other sources, since many of the components (particularly those not being “starting materials”) have not been identified and, thus, not toxicologically evaluated. Finally, attitudes towards different types of food contaminants are divergent, also reflected by the legal measures: for most sources of food contamination there are strict rules calling for minimization, whereas the European packaging industry has even requested a further increase in the tolerance to as close as possible to the limit set by the toxicologists. This paper calls for a more realistic perception and more coherent legal measures—and improvements in the control of migration from packaging material.

On-line coupled high performance liquid chromatography–gas chromatography for the analysis of contamination by mineral oil. Part 1: Method of analysis

For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition.

On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 2: migration from paperboard into dry foods: interpretation of chromatograms.

Mineral oil hydrocarbons are complex as well as varying mixtures and produce correspondingly complex chromatograms (on-line HPLC-GC-FID as described in Part 1): mostly humps of unresolved components are obtained, sometimes with sharp peaks on top. Chromatograms may also contain peaks of hydrocarbons from other sources which need to be subtracted from the mineral oil components. The review focuses on the interpretation and integration of chromatograms related to food contamination by mineral oil from paperboard boxes (off-set printing inks and recycled fibers), if possible distinguishing between various sources of mineral oil. Typical chromatograms are shown for relevant components and interferences as well as food samples encountered on the market. Details are pointed out which may provide relevant information. Integration is shown for examples of paperboard packaging materials as well as various foods. Finally the uncertainty of the analysis and limit of quantitation are discussed for specific examples. They primarily result from the interpretation of the chromatogram, manually placing the baseline and cuts for taking off extraneous components. Without previous enrichment, the limit of quantitation is between around 0.1 mg/kg for foods with a low fat content and 2.5 mg/kg for fats and oils. The measurement uncertainty can be kept clearly below 20% for most samples.

Efficiency through combining high-performance liquid chromatography and high resolution gas chromatography: progress 1995–1999

Progress during the last 5 years in on-line LC-GC and related techniques is reviewed. In normal-phase LC-GC, the wire interface proved to have advantages over the loop type interface. Further investigations on the solvent evaporation process in an uncoated precolumn under conditions of an early vapour exit revealed that the rules for the transfer by the retention gap techniques must be modified. For reversed-phase LC-GC, approaches with a phase transfer compete with direct evaporation. Eluents were extracted into a bed of Tenax located in a programmed-temperature vaporiser and thermally desorbed. Direct evaporation is possible when a hot vaporising chamber is used and solvent/solute separation occurs in a separate compartment, a coated precolumn possibly in combination with packed beds. As a future strategy, LC-GC transfer techniques should be adjusted to those of large volume injection and involve a single device. It is believed that on-column injection/transfer is the choice. This requires that concurrent evaporation in LC-GC is performed by the on-column interface.

Contamination of animal feed and food from animal origin with mineral oil hydrocarbons

Oils and fats used for the production of animal feed can become contaminated with mineral oil material originating from gas oils (C18-C35) or synthetic oils (poly alpha olefins, C25 to beyond C45). An important cause is assumed to be the discharge of waste oils, such as motor oil and hydraulic oils. Mineral oil material was analysed by on-line LC-GC-FID directly in the fat or in a raw extract from animal feed or foodstuffs. In Switzerland in summer/autumn 1999 concentrations in oils and fats for feed production were often found to be between 100 and 1000mg/kg. In the feeds, the average concentration was around 100mg/kg with values ranging up to a maximum of 1000mg/kg; few samples were free of contamination. In animal body fat, the average concentration determined in summer 1999 was 25mg/kg, with a maximum of 150mg/kg, although in samples from December 1999, contamination was substantially lower. In the fat phase of eggs, the average concentration was 30mg/kg, with a maximum of 80mg/kg. Paraffin oil is used for feed production, which may account for part of the contamination problem (e.g. eggs).

Acrylamide in fried and roasted potato products: A review on progress in mitigation

The workshop of the European Commission and the Confederation of the Food and Drink Industries of the European Union (CIAA) held in March 2006 in Brussels, Belgium, discussed the key knowledge and achievements in the mitigation of acrylamide. This paper presents the progress made by the potato sector and identifies areas for future research. Because of the important contribution of potato products to acrylamide intake, it is an area that has received much attention. The discovery of the method of formation and the role of reducing sugars meant that long-standing knowledge in respect of sugar and fry colour could be used to identify methods of mitigation. Improvement in parameters such as (1) potato variety, (2) potato storage temperature, (3) process control (thermal input, pre-processing), (4) final preparation, and (5) colour have all contributed to a significant overall reduction in the average acrylamide content in French fries and potato crisps (termed ‘chips’ in the USA). There is evidence that the limit of reduction that these measures can offer for crisps has now been approached, but clearly more can be done for French fries and roasted potato products. The use of asparaginase offers potentially significant reduction in certain prefabricated potato products. More research is required into new potato varieties and the agronomical factors that influence the levels of asparagine and sugars in potatoes.

Compositional GC-FID analysis of the additives to PVC, focusing on the gaskets of lids for glass jars

A gas chromatographic (FID) method is described which aims at the quantitative compositional analysis of the additives in plasticized PVC, particularly the plastisols used as gaskets for lids of glass jars. An extract of the PVC is analysed directly as well as after transesterification to ethyl esters. Transesterification enables the analysis of epoxidized soya bean and linseed oil (ESBO and ELO) as well as polyadipates. For most other additives, the shifts in the chromatogram resulting from transesterification is used to confirm the identifications made by direct analysis. In the gaskets of 69 lids from the European market used for packaging oily foods, a broad variety of plastisol compositions was found, many or possibly all of which do not comply with legal requirements. In 62% of these lids, ESBO was the principal plasticizer, whereas in 25% a phthalate had been used.

Memory effects with the on-column interface for on-line coupled high performance liquid chromatography-gas chromatography: The Y-interface

When using the on-column interface for on-line high performance liquid chromatography (HPLC)-gas chromatography (GC), there is a memory effect typically equivalent to 0.5-3% of the previous transfer. The shape of peaks distorted as a result of incomplete reconcentration of the initial bands enabled mapping of the distribution of the solute material in the uncoated precolumn and deriving the mechanism which causes the memory effect. The relatively slow transfer of HPLC eluent causes liquid being sucked backwards into the narrow interspace between the transfer line and the precolumn wall. Solvent is evaporated into the passing carrier gas and is replaced by more eluent pulled into this zone, resulting in enrichment of solute material. At the end of the transfer, some of this solute material enters the transfer line and remains there up to the subsequent transfer of an HPLC fraction. This problem is avoided by replacing the on-column injector used as interface by a Y-piece in which the eluent flow from HPLC and the carrier gas are joined. The memory effect was reduced to below 0.02%.

The migration from the internal coatings of food cans; summary of the findings and call for more effective regulation of polymers in contact with foods : a review

The analysis of migrates from the internal coatings of food cans showed that the present regulation is not sufficient to ensure safety of food contact polymers. The migrates often consist of complex mixtures of reaction products and impurities, and their harmlessness cannot be deduced from the use of non-toxic starting substances compiled in positive lists. The regulation proposed herein asks producers to analyse the composition of the migrates. It includes an upper limit for the molecular weight (e.g. 1000 Da) and thresholds defining concentrations in the foods down to which components must be identified and evaluated. Primarily considering feasibility at reasonable costs, thresholds of 30 micrograms/kg for individual components and 300 micrograms/kg for the sum of the unidentified materials are proposed. Producers must be able to demonstrate that the individual components or mixtures exceeding this limit, including reaction products with food components, have no toxic effect.