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Preface Capillary Gas Chromatography Fundamental Aspects Separation System Considerations Analysis of Food Ingredients Components in Food with High Carbohydrate Fats and Compounds in Fat Containing Foods Aroma Compounds Stereodifferentiation of Chiral Flavor and Aroma Compounds High Molecular Weight Compounds Analysis of Residues and Contaminants Pesticide Analysis Contaminant Analysis Headspace Gas Chromatography of Highly Volatile Compounds

Aluminium is one of the most abundant elements in earth’s crust and its manifold uses result in an exposure of the population from many sources. Developmental toxicity, effects on the urinary tract and neurotoxicity are known effects of aluminium and its compounds. Here, we assessed the health risks resulting from total consumer exposure towards aluminium and various aluminium compounds, including contributions from foodstuffs, food additives, food contact materials (FCM), and cosmetic products. For the estimation of aluminium contents in foodstuff, data from the German “Pilot-Total-Diet-Study” were used, which was conducted as part of the European TDS-Exposure project. These were combined with consumption data from the German National Consumption Survey II to yield aluminium exposure via food for adults. It was found that the average weekly aluminium exposure resulting from food intake amounts to approx. 50% of the tolerable weekly intake (TWI) of 1 mg/kg body weight (bw)/week, derived by the European Food Safety Authority (EFSA). For children, data from the French “Infant Total Diet Study” and the “Second French Total Diet Study” were used to estimate aluminium exposure via food. As a result, the TWI can be exhausted or slightly exceeded—particularly for infants who are not exclusively breastfed and young children relying on specially adapted diets (e.g. soy-based, lactose free, hypoallergenic). When taking into account the overall aluminium exposure from foods, cosmetic products (cosmetics), pharmaceuticals and FCM from uncoated aluminium, a significant exceedance of the EFSA-derived TWI and even the PTWI of 2 mg/kg bw/week, derived by the Joint FAO/WHO Expert Committee on Food Additives, may occur. Specifically, high exposure levels were found for adolescents aged 11–14 years. Although exposure data were collected with special regard to the German population, it is also representative for European and comparable to international consumers. From a toxicological point of view, regular exceedance of the lifetime tolerable aluminium intake (TWI/PTWI) is undesirable, since this results in an increased risk for health impairments. Consequently, recommendations on how to reduce overall aluminium exposure are given.

Die Authentizitatsprufung von Lebens- und Futtermitteln umfasst eine grose Bandbreite an Fragestellungen, Matrizes, analytischen Techniken und Forschungsansatzen, weshalb die Vernetzung von offentlichen Instituten eine immer grosere Rolle spielt. Um den Austausch zwischen Experten auf eine breitere Basis zu stellen, organisierte das Bundesinstitut fur Risikobewertung (BfR) erstmals eine bundesweite Veranstaltung fur offentliche Institute mit dem Titel „Status quo der Authentizitatsprufung von Lebens- und Futtermitteln - Analytische Routineverfahren und Forschungsansatze“. Auf Einladung des BfR berichteten Expertinnen und Experten diverser Einrichtungen des Bundes, der Landesuberwachungsbehorden und Universitaten am 13. und 14. Juni 2016 in den Tagungsraumen des BfR uber ihre bisherigen Erfahrungen und Aktivitaten in der Echtheitsuberprufung – Authentizitatsprufung – von Lebens- und Futtermitteln. Das Ziel des BfR, mit dieser Veranstaltung den wissenschaftlichen Austausch in diesem aktuellen Forschungsgebiet durch den Aufbau eines Expertennetzwerkes zu fordern, wurde erreicht.

Environmental emissions of organic contaminants are caused by man-made and natural combustion processes, industrial production facilities, and the release from products. Food represents the main source of human exposure for some of these compounds. This is the case for three groups of persistent organic contaminants: (1) per- and polyfluoroalkyl substances (PFAS), (2) polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), polychlorinated biphenyls (PCBs), and for (3) polycyclic aromatic hydrocarbons (PAHs). The issues regarding PCDD/F emissions were already recognized as a problem in the 1970s and have since then been effectively regulated; the impact of PFAS as global anthropogenic environmental contaminants was identified much later.A system of toxicity equivalency factors (TEF system) was established for the assessment of the toxic potency of a mixed exposure to PCDD/F and certain PCBs. For the health assessment and regulation of PAHs and PFAS, no such system has been implemented so far. For PFAS, a re-evaluation of the present tolerable daily intake values (TDI values) is currently being discussed, as new insights into toxicology and epidemiology have been gained.The persistence in the environment of the compound groups discussed here leads to entry into the food chain over long periods of time, even if access into the environment is minimized. This requires a long-term continuation of the monitoring of food stuffs and forward-looking risk assessment approaches and regulatory measures.

One of the most challenging analytical issues in terms of wine authenticity is the control of geographical origin. This question becomes more and more important in the current context of a global wine market. Single parameters are often not sufficient on their own to determine the product identity with respect to the wine labelling. Recent developments have shown that control is improved by application of multivariate statistical methods to a combination of composition and isotopic data. In the past years, the official European wine control bodies have been confronted with wines that have had to be judged as suspicious in terms of their sophisticated authenticity, falsifications which are not readily identifiable, especially as it regards the grape variety, and particularly highlighted here the geographical origin. To improve the measures of authenticity control, a project with the title “Establishing of a WINE Data Bank for analytical parameters for wines from Third countries (WINE-DB project, G6RD-CT-2001-00646-WINE-DB)” was initiated in 2002, funded by the European Commission within the fifth framework “Competitive and Sustainable Growth”. The project consortium of this multinational project was composed of official and private laboratories from the European Union, from new European member states and a group of university partners for the statistical evaluation. Within the framework of the WINE-DB project, commercial and authentic wines originating from new European member states (Czech Republic, Hungary and Romania) and from overseas countries (South Africa and Australia) are collected and analysed. More than 1,800 wines from three vintages were analysed. First, a sampling plan for each wine-producing country was developed for the authentic samples taking into account, the surface and the grape variety of wine in the respective country. This sampling plan was used for the commercial samples accordingly. A series of three publications was prepared covering the statistical approaches and the results obtained for authentication of wine. The actual one—Part I—provides an overview on the structure of the project, the developing of the sampling plan, the strategy of sample collection and the analytical scheme.

The advent of new testing systems and "omics"-technologies has left regulatory toxicology facing one of the biggest challenges for decades. That is the question whether and how these methods can be used for regulatory purposes. The new methods undoubtedly enable regulators to address important open questions of toxicology such as species-specific toxicity, mixture toxicity, low-dose effects, endocrine effects or nanotoxicology, while promising faster and more efficient toxicity testing with the use of less animals. Consequently, the respective assays, methods and testing strategies are subject of several research programs worldwide. On the other hand, the practical application of such tests for regulatory purposes is a matter of ongoing debate. This document summarizes key aspects of this debate in the light of the European "regulatory status quo", while elucidating new perspectives for regulatory toxicity testing.

A new method for the determination of zearalenone in edible oils with size exclusion chromatography (SEC) followed by LC-MS/MS as well as HPLC-FLD was developed and validated. By using the LC-MS/MS determination no further clean up step is necessary after the SEC. The correlation coefficient of 0.999 for the two detection systems is acceptable. In this research 77 edible oils were analyzed. The mean average value of 38 corn germ oils was 169 μg/kg, the maximum value amounted up to 921 μg/kg.

After the publication of high levels of acrylamide (AA) in food, many research activities started all over the world in order to determine the occurrence and the concentration of this substance in various types of food. As no validated methods were available at that time, interlaboratory studies on the determination of AA in food were of the highest priority. Under the boundary conditions of applying well-established evaluation schemes, the results of 2 studies conducted by the Federal Institute for Risk Assessment (BfR) in Germany and by the European Commission's Directorate General Joint Research Center (JRC) exhibited an overall acceptable performance of the participants in these studies. Nevertheless, many laboratories showed problems in determining AA in food with a complex matrix such as cocoa. The results of analysis also showed a broader variation of AA for samples with low AA concentrations and indicated a bias of the results obtained by gas chromatography–mass spectrometry without derivatization. Improvements of the performance of some laboratories appeared to be necessary.

As a basis for the collection of occurrence and exposure data of ergot alkaloids in food, an HPLC method coupled with fluorimetric detection (HPLC-FLD) for the determination of 12 pharmacologically active ergot alkaloids in rye and rye products was developed. Samples were extracted with a mixture of ethyl acetate, methanol, and aqueous ammonia, followed by centrifugation and purification by solid phase filtration (SPF) with basic alumina. After solvent adjustment, the samples were analyzed by HPLC-FLD using a phenyl-hexyl-column. Recoveries for five major alkaloids were between 89.3% (ergotamine) and 99.8% (alpha-ergokryptine) with a maximum LOQ of 3.3 microg/kg (ergometrine). Precision expressed as RSD ranged from 2.8% (ergocristine) to 12.4% (alpha-ergokryptine) for repeatability, and from 6.5% (ergocornine) to 14.9% (ergotamine) for within-laboratory reproducibility, respectively. In a survey of 39 rye product samples, ergocristine and ergotamine were found to be the major alkaloids in commercially available rye products with contents of 127 microg/kg (ergocristine), and 134 microg/kg (ergotamine) in rye flour, and 152.5 and 117.8 microg/kg in coarse meal, respectively.

A number of zero tolerance provisions are contained in both food and animal feed law, e.g. for chemical substances whose occurrence is not permitted or is directly prohibited in food or animal feed. In the European Union, bans of this kind were introduced to give consumers and animals the greatest possible protection from substances with a possible hazard potential within the intendment of the hazard prevention principles and current precautionary measures. This also applies to substances for which an acceptable daily intake cannot be derived and a maximum residue limit cannot, therefore, be established, e.g. due to missing or inadequate toxicological data. Zero tolerances are also under discussion as trade barriers because their use has triggered numerous legal disputes. This paper draws together the results of an evaluation of alternative risk assessment methods to be used for the risk assessment of substances to which currently only zero tolerances apply. It will demonstrate that, depending on the available toxicological data, a scientifically sound risk assessment may still be possible. In this context, the two concepts - margin of exposure and threshold of toxicological concern - are very promising approaches. Until the scientific and sociopolitical discussions have been completed, it is essential that the principle of zero tolerances be upheld, especially for those substances which may be genotoxic carcinogens. In microbiology, there is no legal room for manoeuvre with regard to food safety criteria established for reasons of consumer health protection on the basis of scientific assessments.

The aim of the present study was to provide the official wine control authorities with an internationally validated method for the determination of 3-methoxy-1,2-propanediol (3-MPD) and cyclic diglycerols (CycDs)-both of which are recognized as impurities of technical glycerol-in different types of wine. Because glycerol gives a sweet flavor to wine and contributes to its full-body taste, an economic incentive is to add glycerol to a wine to mask its poor quality. Furthermore, it is known that glycerol, depending on whether it is produced from triglycerides or petrochemicals, may contain considerable amounts of 3-MPD in the first case or CycDs in the second. However, because these compounds are not natural wine components, it is possible to detect glycerol added to wine illegally by determining the above-mentioned by-products. To this end, one of the published methods was adopted, modified, and tested in a collaborative study. The method is based on gas chromatographic/mass spectrometric analysis of diethyl ether extracts after salting out with potassium carbonate. The interlaboratory study for the determination of 3-MPD and CycDs in wine was performed in 11 laboratories in 4 countries. Wine samples were prepared and sent to participants as 5 blind duplicate test materials and 1 single test material. The concentrations covered ranges of 0.1-0.8 mg/L for 3-MPD and 0.5-1.5 mg/L for CycDs. The precision of the method was within the range predicted by the Horwitz equation. HORRAT values obtained for 3-MPD ranged from 0.8 to 1.7, and those obtained for CycDs ranged from 0.9 to 1.3. Average recoveries were 104 and 109%, respectively.

This article discusses the results of a project funded by the European Commission (EC) Framework IV Standards Measurements and Testing (SMT) Programme to provide official methods for the determination of spirit drinks. The project involved four main partners and over 60 laboratories in the resulting validation studies that evaluated 11 analytical methods, of which 10 were subsequently validated in the four-year study. The methods tested were determinations for: alcoholic strength; total dry extract; volatile acidity; esters; "congeners"; hydrocyanic acid; anethole; glycyrrhizic acid; chalcones; total sugar; and, egg yolk. The majority of the validated methods have been adopted into, or are under discussion for, European Union (EU) legislation. (C) 2003 Elsevier Science B.V. All rights reserved

Within the European Union the determination of chaptalization of wine involves the comparison of the D/H ratios of ethanol with the ratios of authentic wine samples that are similar to the suspect wine in terms of geographical origin, grape variety, and vintage. In the frame of a databank project comparison, wines are produced under official control on a small scale. To clarify the influence of the different production conditions between commercial wines and these databank wines, wines that were produced under varying conditions were investigated by the (2)H NMR method. None of the parameters under investigation, such as yeast strain, fermentation temperature, or wine fining, showed a significant influence on the (D/H)(I) ratio of wine ethanol, which is the most indicative parameter for the determination of the addition of extraneous sugar to wine. For the (D/H)(II) ratio, different values were found for different yeast strains used for fermentation and a slight decrease was observed with increasing fermentation temperature. At increasing points of fermentation yield an increase of the D/H ratios was found in the present alcohol. The total increase of the (D/H)(I) ratio throughout the fermentation was approximately 1 ppm, so that with a fermentation yield of more than 50% no statistical difference could be observed.

An interlaboratory study of a gas chromatographic (GC) method for the determination of volatile congeners in spirit drinks was conducted; 31 laboratories from 8 countries took part in the study. The method uses GC with flame ionization detection and incorpo rates several quality control measures which permit the choice of chromatographic system and conditions to be selected by the user. Spirit drink samples were prepared and sent to participants as 10 blind duplicate or split-level test materials for the determination of 1,1-diethoxyethane (acetal), 2-methylbutan-1-ol (active amyl alcohol), 3-methylbutan-1-ol (isoamyl alcohol), methanol (methyl alcohol), ethyl ethanoate (ethyl acetate), butan-1-ol (n-butanol), butan-2-ol (sec-butanol), 2-methylpropan-1-ol(isobutyl alcohol), propan-1-ol (n-propanol), and ethanal (acetaldehyde). The precision of the method for 9 of the 10 analytes was well within the range predicted by the Horwitz equation.The precision of the most volatile analyte, ethanal, was just above statistically predicted levels. This method is recommended for official regulatory purposes.

Der wahrend der thermischen Pyrolyse von Holz entstehende Raucherrauch, insbesondere die daraus gewonnenen Raucherpraparate, sind sehr reich an phenolischen Verbindungen. Ihre Mitwirkung an der aromatisierenden und konservierenden Wirkung des Raucherrauches ist bewiesen; sie konnten aber auch cancerogene bzw. cocancerogene Eigenschaften besitzen. Um eine moglichst vollstandige Klarung der Zusammensetzung eines nach einem schonenden Verfahren gewonnenen Phenolextraktes zu ermoglichen, wurden die Phenole mit Hilfe einer Natriumboratlosung in die Mono- und Dihydroxyfraktionen getrennt. Die Untersuchung ihrer Trimethylsilyl-Deriva