Total Diet Studies (TDSs) provide data on the occurrence of substances in commonly consumed foods for dietary exposure assessment. We present data from the BfR MEAL Study, the first full-scale German TDS, for the determination of plasticizers and additives in 226 pooled food samples. A multi-technique approach with matrix-dependent sample preparation, which was comprehensively validated in seven representative food matrices, was applied to the samples of various types of food matrices. This approach features high precision, recovery, and sensitivity, enabling reliable determination of 60 target analytes in all types of food collected in this study. In all samples, at least one of the analytes was detected, and in the majority of samples, at least one of the analytes could be quantified. The content of the ortho-phthalate plasticizers connected to reproductive toxicity and endocrine disrupting properties in the samples was low in most cases. A median of weighed overall content of hazardous phthalates (DEHP, DIBP, DNBP, BBP, DINP) of 15.3 μg DEHP equivalents/kg food suggests that overall exposure would be well below the TDI of 50 μg DEHP equivalents/kg bw/day. Detection frequency and content of some alternative plasticizers and additives were higher (e.g., up to 23,000 and 1300 μg/kg food for DINCH and DEHA). However, the median concentrations of these analytes were much lower: 99 and 56 μg/kg food.

Short-chain (SCCPs) and medium-chain (MCCPs) chlorinated paraffins (CPs) are highly complex mixtures extensively used as flame retardants, plasticizers, and lubricants. Next to the presence in food, CPs were repeatedly detected in food contact materials. Within this product class, beeswax wraps have recently gained popularity as a sustainable alternative to conventional packaging materials. A novel sample clean-up procedure consisting of microwave-assisted extraction, a freezing-out step with acetonitrile, countercurrent chromatography, and adsorption chromatography enabled the quantification of CPs in all samples (n = 26) by GC/ECNIOrbitrap-HRMS. New beeswax wraps (n = 19) contained 0.2-15 (average: 2.8) & micro;g CPs per dm2 beeswax wrap. Used wraps were in the same range except for two samples which showed higher levels (20 and 260 & micro;g/dm2 CPs). This produced evidence that beeswax wraps can sorb high amounts of CPs from contaminated (indoor) environments during storage. Due to the lack of experimental data, a theoretical calculation of the transfer of CPs from beeswax wraps into food shows that these can contribute to human exposure to CPs.

Halogenated natural products (HNPs) are a diverse group of organohalogen compounds, predominantly found in the marine environment. Selected HNPs show structural similarity to persistent organic pollutants (POPs), but data on their occurrence is limited. An analytical method for the detection of 17 commonly reported HNPs, as well as selected POPs, using gas chromatography with electron-capture negative ionisation mass spectrometry (GC/ECNI-MS) was established and validated for salmon and blue mussel. The validation confirmed the applicability of the method with recovery rates and inter-day coefficients of variations of 52–101

The release of 21 elemental ions from lead crystal ware and metallic hip flasks into different food simulants as well as alcoholic beverages was investigated in this study. For this purpose, an ICP-MS method including a sample pre-treatment based on microwave-assisted digestion was developed and validated. Elemental ion release from lead crystal glasses into artificial tap water, 0.5% citric acid solution and white wine, respectively, was only analysed for Pb. Within 24 h, Pb release from crystal glass was shown to increase with time. To account for repeated use, at least three consecutive release experiments were performed, which showed - with one remarkable exception - constant or decreasing levels of element ion release. However, after four months resting period, Pb release from crystal glass was higher than before. In contrast, all 21 elemental ions were detected to be released from the hip flasks into 0.5% citric acid solution, apple liqueur and herb liqueur, respectively. Release of Cd, Cr, Ni, As, TI, Sn and most prominently Pb from hip flasks was in the range of and above the respective release limit (SRL) as set by the Council of Europe (CoE). When focussing on the third repetition, only one out of six hip flasks met the suggested SRL for all determined elements in all test solutions. This demonstrates both, that the SRLs of the CoE can be met and that producers of hip flasks may have to review their manufacturing processes.

Chlorinated paraffins (CPs) are amongst the most discussed polyhalogenated pollutants in recent years. Their ubiquitous occurrence in the environment and especially foodstuff has given rise to concerns about CP uptake levels. Especially animal products and oils, i.e. foodstuff with high fat contents showed comparably high CP contaminations. In this study, nut-nougat and chocolate spread samples (n = 30) from the German market were analyzed on the occurrence of short-chain CPs (SCCPs) and medium-chain CPs (MCCPs) via gas chromatography coupled with electron capture negative ion mass spectrometry (GC/ECNI-MS). Fifteen (= 50%) of the samples contained CPs, with MCCPs being much higher abundant (17-270 ng/g fresh weight (fw)) in most samples than SCCPs (7.5-50 ng/g fw). No statistical correlation could be established between SCCP or MCCP occurrence on one hand and manufacturer or ingredients, such as palm oil on the other hand. A preliminary risk assessment of the detected levels gave margins of exposure (MOE) to CPs from consumption of chocolate and nut-nougat spreads ranging from approx. 16,000 to 48,000. Since health concerns are expected at an MOE of <1,000, this indicated no risk from CP intake for the consumer by consumption of these products, based on current knowledge.

The development of multi-analyte methods is always challenging, especially when the target compounds derive from many different substance classes. We present an approach to analyze up to 60 additives – mainly plasticizer – including 28 phthalates and 32 further compounds such as sebacates, adipates, citrates, fatty acid amides, among others. Our multi-analyte multi-technique approach combines a single sample preparation step with one GC-MS/MS and two LC-MS/MS quantification methods. We demonstrate the applicability for beverages by a full validation in tomato juice matrix and determining the recoveries in apple juice, mulled wine, and spirits. The approach features good reproducibilities and high precisions with limits of quantification in the low µg·kg−1 food range, enabling the method to be applied for enforcement and especially for exposure investigations. In course of the BfR MEAL study, 16 pooled beverage samples were examined and - if at all - analytes were found only in very low concentrations.

The consumption of seafood containing marine biotoxins called ciguatoxins (CTXs) can result in ciguatera poisoning (CP), a globally prevalent seafood-born human illness. The southwestern coast of India is a regional source of seafood attributed to isolated and mass outbreaks of CP since 2015, both locally and exported globally. Samples of frozen snapper product (Lutjanus bohar) described herein, were part of a 7000 kg international shipment into the European Union from southwest India and implicated in a CP outbreak in the Netherlands. DNA barcoding confirmed the species as Lutjanus bohar with a base pair identity of 99%. LC-MS/MS and HRMS analyses describe CTX-3C-group compounds with an in vitro Neuro-2a (cell-based) cytotoxicity MTT-assay based toxicity range of 0.79-5.39 ng CTX-3C equivalent (eq.) per g wet tissue eq. This CP traceback includes an investigation and description of the production chain distribution, catch region, outbreak, toxin-group, and follow-up actions for the seafood products associated with the outbreak. Together this in-depth traceback investigation provides an account of the CP outbreak from harvest to consumption for a region of coastal India with a sizable seafood production industry but with limited CP data.

Progressive climate change holds the potential for increasing human health risks from waterborne infections and intoxications, e. g. through an increase in pathogen concentrations in water bodies, through the establishment of new pathogens or through possible changes in pathogen properties. This paper presents some examples of potential impacts of climate change in Germany. Non-cholera Vibrio occur naturally in seawater, but can proliferate significantly in shallow water at elevated temperatures. In the case of Legionella, climate change could lead to temporary or longer-term increased incidences of legionellosis due to the combination of warm and wet weather. Higher temperatures in piped cold water or lower temperatures in piped hot water may also create conditions conducive to higher Legionella concentrations. In nutrient-rich water bodies, increased concentrations of toxigenic cyanobacteria may occur as temperatures rise. Heavy rainfall following storms or prolonged periods of heat and drought can lead to increased levels of human pathogenic viruses being washed into water bodies. Rising temperatures also pose a potential threat to human health through pathogens causing mycoses and facultatively pathogenic micro-organisms: increased infection rates with non-tuberculous mycobacteria or fungi have been documented after extreme weather events.

LebensmittelchemieVolume 77, Issue S3 p. S3-115-S3-115 Analytik Development and Validation of an Optimized Method for the Gravimetric Determination of volatile organic compounds in Silicone-based Consumer Products B. Poelke, B. Poelke Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorA. Kuklya, A. Kuklya Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorO. Krüger, O. Krüger Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorI. Ebner, I. Ebner Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorO. Kappenstein, O. Kappenstein Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorA. Roloff, A. Roloff Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorA. Luch, A. Luch Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorT. Bruhn, T. Bruhn Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this author B. Poelke, B. Poelke Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorA. Kuklya, A. Kuklya Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorO. Krüger, O. Krüger Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorI. Ebner, I. Ebner Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorO. Kappenstein, O. Kappenstein Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorA. Roloff, A. Roloff Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorA. Luch, A. Luch Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this authorT. Bruhn, T. Bruhn Berlin/D Bundesinstitut für Risikobewertung (BfR), Max-Dohrn-Straße 8-10, 10589 Berlin/DSearch for more papers by this author First published: 01 August 2023 https://doi.org/10.1002/lemi.202359096AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onEmailFacebookTwitterLinkedInRedditWechat No abstract is available for this article. References [1] Bundesinstitut für Risikobewertung, BfR Empfehlung XV Silicone, of 01.02.2023, https://www.bfr.bund.de/cm/349/XV-Silicones.pdf, assessed June 2023. [2]O. Krüger, I. Ebner, A. Roloff, O. Kappenstein, T. Bruhn, BfR-Wissenschaft, 2021. [3]O. Krüger, I. Ebner, O. Kappenstein, A. Roloff, A. Luch, T. Bruhn, Food Packag. Shelf Life, 2021, 30, 100758. [4] Bundesinstitut für Risikobewertung, Determination of volatile compounds in silicone consumer products, of 03/2022, https://www.bfr.bund.de/cm/349/determination-of-volatile-compounds-in-silicone-consumer-products.pdf, assessed June 2023. Volume77, IssueS3Supplement: Abstracts der Vorträge, Posterflashtalks und Poster von den 51. Deutschen Lebensmittelchemietagen 2023August 2023Pages S3-115-S3-115 ReferencesRelatedInformation

Polyamides (PAs) are types of polymers used as food contact materials (FCMs) and articles such as kitchen utensils and packaging material. While caprolactam is an EU regulated substance and monomer of PA, this material's oligomers are instead considered as non-intentionally added substances (NIAS) and are typically found in PA-based packaging. An analytical methodology was developed and validated for the quantification of both monomers and oligomers of PA in official liquid food simulant (simulant A;10% v/v ethanol), using a quadruple time-of-flight mass spectrometer (QTOF-MS). The method was applied in the evaluation of the effect of the ionic strength on the migration of all the studied monomers and oligomers from a PA/polyethylene FCM multilayer film. The migration experiments results at different conditions (temperature, time) and with different concentration (% w/v) of NaCl, showed ranging values for the PA6 oligomers (trimer up to heptamer) and caprolactam. It was observed that in the presence of salt, the mass fractions of the migrated caprolactam, were above the limits specific in the respective EU regulation. Preliminary results seem to suggest that migration testing should consider not only the fatty content of a food, but also its salt content, as changes in the ionic strength may influence the migration of polar substances.

Ciguatera poisoning (CP) is a prevalent food related health risk, caused by the consumption of seafood contaminated with ciguatoxins (CTXs). Seafood is the most traded food commodity worldwide, and since 2012, imported snapper fish (Lutjanidae) were the leading cause of CP in Germany. Following a Germany wide CP outbreak in 2017, a product trace-back investigation was conducted for imported fish labeled as “Red Snapper” (Lutjanus malabaricus). Forty-five fish muscle-tissue portions from the implicated batch and two meal remnants were analyzed for CTXs. All samples were positive for “CTX-like toxicity” containing a range of 0.23–11.4 ng CTX3C equivalents per gram of wet tissue, determined by an in vitro cell assay [N2a-3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT)]. Liquid chromatography with tandem mass spectrometry (LC-MS/MS) chromatograms revealed the (potential) presence of several marine biotoxins of the class CTX in all batch samples. All samples exceeded current multi-national product legal requirements and recommended guidelines for CTXs. DNA barcoding confirmed the fish sold was mislabeled and was identified as L. bohar, a species frequently involved in CP. Consequently, the mislabeled food and contaminants risk focuses attention on the importance of correct food labeling. Processes for food authentication and CTX contaminant analysis exist and can be used to potentially prevent, stop, and remove foods from commerce for further evaluation to ensure consumer safety. This study further demonstrates their necessity.

Abstract The consumption of seafood containing marine biotoxins called ciguatoxins (CTXs) can result in ciguatera poisoning (CP), a globally prevalent seafood-born human illness. Since 2015 isolated and mass outbreaks of CP have occurred along the southwestern coast of India, however, no attributable CTXs have yet been identified. Herein, several CTXs are described in an often marketed snapper species (Lutjanus bohar) from southwest India. CTX3C-group compounds were identified by LC-MS/MS with a toxicity range of 0.79-5.39 ng CTX3C equivalent (eq.) g-1 wet tissue eq., as determined by an in vitro cell (Neuro-2a) assay. Samples investigated were part of a 7,000 kg international shipment of frozen snapper product imported into the European Union and subsequently implicated in a 2020 CP outbreak in the Netherlands. The identification of CTX3C-group toxins in fish originating from coastal India suggests a re-evaluation of the current understanding of CTXs associated CP with seafood from the Indian Ocean region.

Ciguatoxins (CTXs) are a group of marine biotoxins, consisting of over 30 different congeners that can contaminate marine food webs. Generally, the molecular structures among the known congeners are variable by geographical region (i.e., ocean basin) and vector species. Limited information is available regarding the CTX profiles among or within CTX vector species and their capture regions. Within this study, an in-depth investigation based on a semi-targeted LC-MS/MS approach was conducted to investigate 52 tissue samples from a single species Lutjanus bohar (Lutjanidae), a common CTX vector, sourced from two distinct regions (Indian Ocean and Pacific Ocean). All samples revealed the presence of a complex CTX contaminant profile, with samples containing several congeners of the CTX3C-group (2,3,51-trihydroxyCTX3C, 2,3,-dihydroxyCTX3C, 2-hydroxyCTX3C, M-seco-CTX3C, 51-hydroxyCTX3C, CTX3C, and respective 49-epimers in most cases). All samples were previously found to possess a CTX-like toxicity within an in vitro cytotoxicity assay (N2a-bioassay), demonstrating the relevance of CTX3C-group congeners with regard to ciguatera poisoning. Individual samples contained an indistinguishable toxin profile within the species and among the distinct oceanic capture regions. These findings imply either a species-specific CTX metabolism or the emergence of an interoceanic CTX toxin profile. The inter-regional CTX profile demonstrated here provides further evidence that classifying CTX congeners based on ocean basins may be imprecise.

Lupin varieties with a low content of quinolizidine alkaloids (QAs) like blue sweet lupin (BSL) have long been used as a protein source for dairy cows. A health concern for humans may arise from the transfer of acute toxic QAs from feed into cow's milk. This study is the first to quantify the transfer of QAs from BSL into cow's milk with experimental and modeling methods. Four lactating dairy cows were subjected to two 7 day feeding periods with 1 and 2 kg/d BSL, respectively, each followed by a depuration period. BSL contained 1774 mg/kg dry matter total QAs. Individual milk samples were taken twice daily and QA contents in feed and milk determined with liquid chromatography-tandem mass spectrometry. Transfer of QAs into the milk was already seen with the administration of 1 kg/d BSL, with differences in transfer rates (TRs) between individual QAs. A toxicokinetic model was derived to quantify and predict QA feed-to-food transfer. For the four most prominent QAs, our model shows an alpha-half-life of around 0.27 d. TRs were obtained for six QAs and were between 0.13 (sparteine) and 3.74% (multiflorine). A toxicological assessment of milk containing QAs as measured in this study indicated a potential health concern.

Silicone-based consumer products may contain volatile compounds, predominantly residual siloxane oligomers from production processes. To avoid unwanted release of these volatiles into food, postproduction removal by a tempering process is necessary and might be mandatory for consumer products - especially food contact materials (FCM). According to BfR recommendation XV tempering is assumed to be sufficient if the remaining volatile organic compounds (VOCs) represent less than 0.5 % of the total product weight, a value chosen 60 years ago indicating good manufacturing practice (GMP). However, the reproducibility and comparability of the respective gravimetric method results may be affected by several parameters including sample conditioning, ventilation in the oven and speed of sample handling. Based on the investigations reported in this work, a method evaluation study with an optimized and in-house validated procedure was conducted to assess its inter-laboratory reproducibility. According to the results, the gravimetric determination of the loss of volatile compounds is feasible with an expanded measurement uncertainty of 25 %.

Elastomers are not a uniform class of materials but comprise a broad spectrum of chemically different polymers. Sealing gaskets, gloves, teats, conveyor belts and tubing are examples of elastomers being used as food contact materials (FCMs). Ten elastomer samples were evaluated with respect to the content of extractable compounds, migration of substances into ethanolic food simulants, swelling in food simulants and release of elements in different food simulants. The number of extractable substances <1000 Da was determined by comprehensive two-dimensional gas chromatography coupled with flame ionisation detection (GC × GC–FID) analysis of tetrahydrofuran (THF) extracts. The number of signals ranged from 61 (a thermoplastic elastomer (TPE)) to 690 (a natural rubber/styrene-butadiene-rubber blend (NR/SBR)). As for risk assessment, the decisive factor is which substances reach the food. The extent of substances that migrate into ethanolic food simulants was investigated. Elastomer FCMs can be the source of food contamination with heavy metals. Notably, contamination with lead was detected in some samples investigated in this study. It was shown that food simulants harbour the potential to morphologically alter or even disintegrate elastomeric materials. The results presented here highlight the importance to carefully choose the elastomer type for the intended use as FCMs as not every application may prove safe for consumers.

Globally, the livelihoods of over a billion people are affected by changes to marine ecosystems, both structurally and systematically. Resources and ecosystem services, provided by the marine environment, contribute nutrition, income, and health benefits for communities. One threat to these securities is ciguatera poisoning; worldwide, the most commonly reported non-bacterial seafood-related illness. Ciguatera is caused by the consumption of (primarily) finfish contaminated with ciguatoxins, potent neurotoxins produced by benthic single-cell microalgae. When consumed, ciguatoxins are biotransformed and can bioaccumulate throughout the food-web via complex pathways. Ciguatera-derived food insecurity is particularly extreme for small island-nations, where fear of intoxication can lead to fishing restrictions by region, species, or size. Exacerbating these complexities are anthropogenic or natural changes occurring in global marine habitats, e.g., climate change, greenhouse-gas induced physical oceanic changes, overfishing, invasive species, and even the international seafood trade. Here we provide an overview of the challenges and opportunities of the 21st century regarding the many facets of ciguatera, including the complex nature of this illness, the biological/environmental factors affecting the causative organisms, their toxins, vectors, detection methods, human-health oriented responses, and ultimately an outlook towards the future. Ciguatera research efforts face many social and environmental challenges this century. However, several future-oriented goals are within reach, including digital solutions for seafood supply chains, identifying novel compounds and methods with the potential for advanced diagnostics, treatments, and prediction capabilities. The advances described herein provide confidence that the tools are now available to answer many of the remaining questions surrounding ciguatera and therefore protection measures can become more accurate and routine.

Chlorinated paraffins (CPs) have been repeatedly detected in the kitchen environment. Especially baking ovens were contaminated with high CP amounts on the insides of the doors. To investigate if CPs could be transferred into baked food, we spiked self-synthesized single chain C12-CP and C15-CP standards onto the inside door of an unused, CP-free baking oven. Experiments were performed under different conditions to assess possible CP transportation pathways. Coconut fat was used as food simulant, the exhaust air was monitored with cellulose filter paper and remaining CPs were collected via cotton wipes. In all experiments, both C12- and C15-CPs could be identified in both the food simulant and the cellulose samplers. Mean transfer rates into the food simulant amounted to 2.2% for C12-CPs and 5.8% for C15-CPs. Baking of food in CP-containing baking ovens may perceptibly increase the CP intake of consumers.