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This research presents an analytical technology for highly efficient, high-resolution, and high-yield fractionation of compounds after gas chromatography (GC) separations. The technology is straightforward, does not require sophisticated cold traps or adsorbent traps, and allows collecting large numbers of fractions during a GC run. The technology is based on direct infusion of a carrier solvent at the end of the GC column, where infusion takes place in the GC oven. Pentane and hexane used as carrier solvent showed good results. Acetonitrile also showed good results as a more polar carrier solvent. Development and optimization of the technology is described, followed by demonstration in a high-throughput effect directed analysis setting toward dioxin receptor bioactivity. The GC fractionation setup was capable of collecting fractions in the second range. As a result, fractionated compounds could be collected into one or two fractions when 6.5 s resolution fractionation was performed. Subsequently, mixtures containing polycyclic aromatic hydrocarbons, of which some are bioactive toward the dioxin receptor, were profiled with a mammalian gene reporter assay. After fractionation into 96-well plates, we used our new approach for direct cell seeding onto the fractions prior to assaying which allowed dioxin receptor bioactivity to be measured directly after fractionation. The current technology represents a great advance in effect directed analysis for environmental screening worldwide as it allows combining the preferred analytical separation technology for often non-polar environmental pollutants with environmentally relevant bioassays, in high resolution.

The shortage of data on non-intentionally added substances (NIAS) present in food contact material (FCM) limits the ability to ensure food safety. Recent strategies in analytical method development permit NIAS investigation by using chemical exploration, but this has not been sufficiently investigated in risk assessment context. Here, exploration is utilized and followed by risk prioritization on chemical compounds that can potentially migrate to food from two paperboard FCM samples. Concentration estimates from exploration are converted to tentative exposure assessment, while predicted chemical structures are assessed using quantitative structure-activity relationships (QSAR) models for carcinogenicity, mutagenicity, and reproductive toxicity. A selection of 60 chemical compounds from two FCMs is assessed by four risk assessors to classify compounds based on probable risk. For almost 60% of cases, the assessors classified compounds as either high priority or low priority. Unclassified compounds are due to disagreements between experts (18%) or due to a perceived lack of data (23%). Among the high priority substances are high-concentration compounds, benzophenone derivatives, and dyes. The low priority compounds contained e.g. oligomers from plasticizers and linear alkane amides. The classification scheme provides valuable information based on tentative data and is able to prioritize discovered chemical compounds for pending risk assessment.

In fields such as food safety and environmental chemistry, ensuring safety is greatly challenged by large numbers of unknown substances occurring. Even with current state-of-the-art mass spectrometers, dealing with nonidentified substances is a very laborious process as it includes structure elucidation of a vast number of unknowns, of which only a fraction may be relevant. Here, we present an exploration and prioritization approach based on high-resolution mass spectrometry. The method uses algorithm-based precursor/product-ion correlations on quadrupole time-of-flight tandem mass spectrometry data to retrieve the most likely chemical match from a structure database. In addition, time-of-flight-only data are used to estimate analyte concentration via semiquantification. The method is demonstrated in recycled paper food contact material. Here, 585 chromatographic peaks were discovered, of which 117 were unique to the sample and could be tentatively elucidated via accurate mass, isotopic pattern, and precursor/product-ion correlations. Nearly 85% of these 117 peaks were matched with database entries, which provided varying certainty of information about the analyte structure. Semiquantitative concentration ranges of investigated compounds were between 0.7 and 1600 μg dm . With these data, a subgroup of chemicals was risk-categorized and prioritized by using the most likely candidate structure(s) obtained. Prioritization based on expected health impact was possible by using the tentatively assigned data. Overall, the described method not only is a valuable chemical exploration tool for nonidentified substances but may also be used as a preliminary prioritization tool for substances expected to have the highest health impact, for example, in food contact materials.

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In this study we compare two parallel analytical methods while also testing a microplastics mitigation method. We assess the effectiveness of a bubble curtain to reduce microplastics in a wastewater treatment plant (WWTP)-effluent canal during the course of six months (> 70 samples) using two analytical techniques: laser direct infrared (LDIR) and optical microscopy (OM) covering a size range of 0.02 to 5 mm. Comparison of the two analytical strategies shows similar trends, fluctuations, and correlating particle and fibre numbers. However, absolute values of particles differ, and the strategies provide different levels of information: LDIR is capable of identifying the plastic type as well as shape, while OM cannot determine the plastic type. Furthermore LIDR has a lower size limit (10–20 μm) than OM (50 μm). While information obtained by OM in general is far less detailed it is more affordable. This research also shows that the bubble curtain pilot does not have a measurable effect on the particle concentration. Possible effects of the curtain are hidden in the temporal variations. This research also reveals that individual samples show a large variation in particle numbers, illustrating that single measurements might give a poor representation of environmental particle number.

In this month's Featured Article Eelco Pieke and his colleagues from the National Food Institute, Technical University of Denmark, discuss some timely issues in the objective and practical assessment of food and environmental safety. As the authors rightly suggest, in our increasingly unpredictable world, even with powerful analytical tools at our disposal, the realistic assessment of risk is a challenge. In any given scenario, an almost limitless array of unknown substances can ‘contaminate’ our environment, and depending on structure, properties and amount, any one of these could pose a significant threat. The task of defining the risk in a cost‐ and time‐efficient manner is much more than an exercise in analytical chemistry given the volume of data, scope of the problem and the uncertainties involved. In this article Pieke, Smedsgaard and Granby discuss their approach to defining and prioritizing risk. They use mass spectrometry as their central analytical platform for both structural elucidation and to estimate analyte concentration and they illustrate their approach through a practical, real‐world example involving food contact materials.