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Background In recent years there have been significant advancements in the understanding of mineral oil hydrocarbons (MOH) in foods and their potential risk to health. However, important gaps in knowledge remain, such as the lack of validated and standardized analytical methods for relevant food matrices and gaps in assessing the risk for consumers’ health. Scope & approach A workshop was organized by the European Branch of the International Life Science Institute to identify knowledge gaps in analytical methods, assessment of exposure, hazard characterisation, and risk assessment of MOH. This work captures the outcome of the workshop and builds upon it by combining the perspectives of the participants with an updated review of the literature to provide a roadmap for future management of the topic. Key findings and conclusions Most participants to the workshop agreed that the key issue underlying many of the knowledge gaps in the field of MOH risk analysis and management is the lack of standardized, validated analytical methods able to assure good inter-laboratory reproducibility and to enable understanding of MOH occurrence in foods. It has been demonstrated that method EN 16995 used for MOH determination in vegetable oils and fats is not reliable below 10 mg/kg of food. There is also a need for confirmatory methods that provide a detailed characterization of the unresolved complex mixture observed from one-dimensional chromatographic methods. This is required to enable adequate substance identification and quantification for input into risk assessment. A major gap in the exposure estimation is the limited number of surveys covering a wide range of foods and enough samples to detect major sources of contamination other than packaging in paperboard. Data on concentration of MOH fractions in human body needed to determine internal exposure estimates is scarce. Data relating concentration in tissues with personal data, lifestyle, food intake and the use of cosmetics are needed to clarify the complex system of distribution of MOSH in the body and to possibly establish relationship between external and internal exposure. Additional toxicological studies to better characterize the hazards of relevant MOH are required for a better human health risk assessment.

The effects of temperature (5 °C, 12 °C, and 21 °C) and time (0 h, 1 h, 3 h, 5 h, 24 h) on the camel cream crystallization mechanisms during ripening were investigated. Particles size, solid fat content (SFC), melting behavior and polymorphism were evaluated. Significant increase of the number of larger droplets was observed for samples ripened at 21 °C as a function of ripening time. Analysis of the solid fat content and the total enthalpy of melting curves indicated that, regardless of the temperature, the crystallization of camel milk cream occurs especially during cooling step and during the first hour of ripening. The results revealed that ripening of camel milk cream at 5 °C and 12 °C promoted a transition from α to β′2 and appearance of β. However, β′1 and β crystals were found in camel cream throughout the ripening at 21 °C. The present study enables a better understanding of the crystallization mechanisms of camel milk cream during ripening, which is needful during the production of butter camel milk.

In the present work, the performance of the multiple-cumulative trapping headspace solid-phase microextraction technique used in the headspace linearity range and saturated headspace was investigated and compared, with the ultimate goal of maximizing the fingerprinting information extractable using a cross-sample comparison algorithm for olive oil quality assessment. It was highlighted as the use of 0.1 g of olive oil provides comparable or even better profiling than 1.5 g at a little expense of sensitivity. However, the use of multiple-cumulative-solid-phase microextraction, along with the correct sample volume, improved not only the overall sensitivity but significantly burst the level of information for cross-sample studies.

The production of renewable fuels as biodiesel and bio-jet fuel is usually originated by the transformation and processing of oleaginous feedstocks, mainly composed of triacylglycerols. Currently, a significant part of the triacylglycerol production relies on grassy oil crops or other woody oil plants, representing more than 120 million metric tons every year. Considering that the worldwide triacylglycerol demand is expected to rise in the future, alternative routes are necessary to ensure a sustainable biodiesel industry and limit diesel price volatility. In this context, the use of animal fats could be an interesting alternative for biodiesel production as the production of animal byproducts represents nearly 17 million tons per year in the European Union only (2020). Animal fats, however, contain large amounts of no-esterified fatty acids and other oxygen compounds, reducing the yield of biodiesel. Therefore, a specific pretreatment is needed before the trans-esterification process. The setup of such appropriate pretreatments requires detailed upstream characterization of the minor components present in the feedstock. For this purpose, the minor component profile of animal fat was investigated by comprehensive two-dimensional gas chromatography coupled with high-resolution time-of-flight mass spectrometry. This was preceded by an innovative sample fractionation and focalization of these minor components by a preparative liquid chromatographic column method. The overall method permitted to extract different levels of information from the two-dimensional chromatograms, leading to a tentative identification of more than 150 compounds, mainly oxygenated, belonging to different chemical classes.

This study aimed to compare the enrichment capacity of polyunsaturated fatty acids (PUFA) and the long chain polyunsaturated fatty acids (LC-PUFA) of two dipteran species, Hermetia illucens - black soldier fly (BSF) - and a blowfly, Chrysomya putoria (CP), and to test its influence on growth, digestive activities and immune responses of Nile tilapia. Two types of enriched insect larval meal were produced using larvae cultured either on vegetable substrates (VGS) to formulate two diets rich in linolenic acid (ALA) (BSF/VGD and CP/VGD), or on fish offal substrates (FOS), in order to produce two diets rich in ALA and eicosapentaenoic acid (EPA) (BSF/FOD) or in ALA + EPA and docosahexaenoic acid (DHA) (CP/FOD). These four insect-based diets containing only palm oil as a lipid source were compared to a control diet based on fish meal (FM) and fish oil (FO). After 60 days of feeding, ALA or DHA muscle content of fish fed BSF/VGD or CP/FOD diet was comparable to that of the FMFO diet, and all insect diets increased the EPA muscle levels, except for a reduction by the BSF/VGD one. The CP/FOD diet induced similar fish growth, feed efficiency and protein efficiency ratio compared to the control FMFO diet, while a decrease was observed in fish fed other insect diets. Only BSF/VGD led to a decrease in protein and lipid digestibility. CP or BSF larval meal significantly increased alkaline phosphatase activity regardless of fatty acid (FA) enrichment. The expression level of fads2, fads6 and elovl5 was significantly higher in fish fed the BSF/VGD diet compared to fish fed the FMFO diet. FA-enriched insect diets increased some immune variables such as lysozyme, peroxidase and ACH50 values of fish fed CP/FOD, CP/VGD or BSF/VGD diets. Moreover, the expression level of β-defensin-1 and mhcII genes were significantly higher in fish fed the BSF/FOD diet than the FMFO diet. Also, the expression of the pro-inflammatory gene il-1-β was significantly higher in fish fed FMFO diet than in those fed CP/FOD diet, but comparable to fish fed all other diets. No significant effects were observed for the other tested genes. The results showed a better efficiency in LC-PUFA enrichment of the CP larvae compared to BSF ones, resulting in a higher stimulation of the fish nutrient utilization processes and therefore, a higher growth capacity. Nonetheless, all dipteran larval meal stimulated the immune status whatever the insect species or dietary essential fatty acids.

The aquaculture sector is expanding rapidly and needs an increasing supply of fishery products. To ensure an ecological transition of this sector, alternative feed ingredients are required for fish nutrition. Potential alternatives include insects, particularly the black soldier fly (BSF, Hermetia illucens L. 1758), which is being increasingly targeted for their nutritional qualities and their sustainable production practices. BSF have a well-balanced amino acid profile; however, their fatty acid profile is not sufficiently balanced for most aquafeed formulations but can be modulated through their feed. In this study, two different batches of BSF prepupae (BSFP) were firstly produced: BSFP with a standard ω3 content (C18:3n-3 ≈ 1.36%) and ω3-enriched BSFP (C18:3n-3 ≈ 9.67%). Then, three isoproteic, -lipidic and -energetic trout feeds were formulated and produced: one control and two feeds containing 75% BSF meal as a substitute for fish meal (standard vs ω3-enriched-BSF). Finally, a trout feeding trial (n = 3 for each feed batch) in a recirculating aquaculture system was carried out for 75 days. BSFP meal inclusion in trout diets did not impact most nutritional and growth parameters of trout compared to the control; however, the coefficient of fatness increased, weight gain decreased and fatty acid profiles of fillets were altered. In conclusion, this study presents a more sustainable model of trout production by including insects from bioconversion of local byproducts in aquafeed.

A high throughput, high-sensitivity procedure, involving simultaneous microwave-assisted extraction (MAS) and unsaponifiable extraction, followed by on-line liquid chromatography (LC)-gas chromatography (GC), has been optimised for rapid and efficient extraction and analytical determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in cereal-based products of different composition. MAS has the advantage of eliminating fat before LC-GC analysis, allowing an increase in the amount of sample extract injected, and hence in sensitivity. The proposed method gave practically quantitative recoveries and good repeatability. Among the different cereal-based products analysed (dry semolina and egg pasta, bread, biscuits, and cakes), egg pasta packed in direct contact with recycled paperboard had on average the highest total MOSH level (15.9 mg kg(-1)), followed by cakes (10.4 mg kg(-1)) and bread (7.5 mg kg(-1)). About 50% of the pasta and bread samples and 20% of the biscuits and cake samples had detectable MOAH amounts. The highest concentrations were found in an egg pasta in direct contact with recycled paperboard (3.6 mg kg(-1)) and in a milk bread (3.6 mg kg(-1)).

Two data elaboration approaches for evaluating olive oils authenticity were compared: (I) determination of the difference between the theoretical and actual amounts of triacylglycerols with partition number 42 (ΔECN42 ⩽ |0.2|); and (II) the global method, which considers also partition numbers 44 and 46 (returning a "correct"/"not correct" result). Analysis of 31 genuine extra virgin olive oil samples was performed using different analytical methods, namely liquid chromatography (LC) coupled with a refractive index detector (RID) and LC coupled with a mass spectrometry (MS), and the results compared. Several false positives were highlighted using the ΔECN42 limit with both instrumental approaches. The global method algorithm returned "correct" results for all the samples analysed (except two that gave no results) with LC-MS; on the other hand, 10 false positives were obtained elaborating data deriving from NARP-LC-RID analysis.

Natural estrogens (estrone: E1, 17β-estradiol: E2, estriol: E3) and the synthetic estrogen (17α-ethinylestradiol: EE2) are endocrine disruptors harmful to aquatic wildlife. The European Commission included these molecules in the surface water Watch Lists issued in 2015 and 2018 under the Water Framework Directive regarding emerging aquatic pollutants, proposing maximum detection limits (LOD) of 0.035 ng/L for EE2 and 0.4 ng/L for E1 and E2. Attaining these limits represents a challenge even with the most up-to-date analytical tools, in particular in surface water. A two-step sample preparation, involving a preliminary extraction of a whole water sample on a solid-phase extraction (SPE) disk and further purification on a Florisil SPE cartridge, was optimized. The purified extract was derivatized subsequently and quantified by LC-MS/MS. The main goal was to maximize the recoveries to achieve the very low LODs required by the European Watch Lists. The method was fully validated in seven surface water. The LODs calculated were below the maximum acceptable limits required by the European Commission.

The present research is focused on the use and evaluation of a novel helium ionization detector, defined as barrier discharge ionization detector (BID), within the context of (low-)flow modulation comprehensive two-dimensional gas chromatography (FM GC × GC). The performance of the BID device was compared to that of a flame ionization detector (FID), under similar FM GC × GC conditions. Following development and optimization of the FM GC × GC method, the BID was subjected to fine tuning in relation to acquisition frequency and discharge flow. Moreover, the BID performance was measured and compared to that of the FID, in terms of extra-column band broadening, sensitivity and dynamic range. The comparative study was carried out by using standard compounds belonging to different chemical classes, along with a sample of diesel fuel. Advantages and disadvantages of the BID system, also within the context of FM GC × GC, are critically discussed. In general, the BID system was characterized by a more limited dynamic range and increased sensitivity, compared to the FID. Additionally, BID and FID contribution to band broadening was found to be similar under the operational conditions applied. Particular attention was devoted to the behaviour of the FM GC × GC-BID system toward saturated and aromatic hydrocarbons, for a possible future use in the field of mineral-oil food contamination research.

Polycyclic aromatic hydrocarbons are ubiquitous compounds, well-known to be carcinogenic, which can reach the food in different ways. Thus the analysis of such compounds has always been of great importance. The aim of the present review, is not only to give an overview of the most recent sample preparation and analytical approaches (such as pressurized liquid extraction, solid-phase microextraction, supercritical fluid extraction, etc.), but also to introduce such a topic to researchers who want to approach it for the first time; therefore, the most significant references related to general aspects, such as formation, toxicity, risk assessment, occurrence in food, are reported and briefly discussed.

The present contribution describes an investigation directed towards the use of a rapid heart-cutting multidimensional LC–GC–FID method for the analysis of mineral oil saturated hydrocarbons (MOSH), contained in different types of homogenized solid baby food (fish, meat and fruit products). The fish and meat products all contained vegetable oil (sunflower), potentially an important source of mineral-oil contamination. Sixteen commercial baby food samples were subjected to analysis, with various degrees of MOSH contamination (from 0.3 mg/kg to circa 14 mg/kg) found. Hence, MOSH contamination was found not only in the meat and fish products, but also in the fruit ones. A fruit-based baby food was lab-made, using the ingredients reported on the commercial product, and was found to be contaminated. The single ingredients were then subjected to LC–GC analysis, with corn starch and sugar found to be the source of contamination. For confirmation of the analytical findings, three of the sixteen samples were analyzed in two separate laboratories, using two distinct LC–GC methods, based on different interfaces. The results were confirmed, in qualitative terms, by collecting the LC fractions, relative to some of the food samples, and subjecting them to comprehensive two-dimensional GC-quadrupole mass spectrometry. Thus, mass spectral data were attained for the saturated hydrocarbons.

The present investigation is focused on a simple flow modulator (FM), for comprehensive two-dimensional gas chromatography (GC×GC). The interface is stable at high temperatures, and consists of a metallic disc (located inside the GC oven) with seven ports, which are connected to an auxiliary pressure source via two branches, to the first and second dimension, to a waste branch (linked to a needle valve) and to an exchangeable modulation loop (2 ports). The ports are connected via micro-channels, etched on one of the inner surfaces of the disc. Modulation is achieved using a two-way electrovalve, connected on one side to the additional pressure source, and to the two metal branches, on the other. An FM enantio-GC×polar-GC method (using a flame ionization detector) was optimized (a 40-μL loop was employed), for the analysis of essential oils. As an example, an application on spearmint oil is shown; the method herein proposed was subjected to validation. Finally, an FM GC×GC diesel experiment was carried out, using an apolar-polar column combination, to demonstrate the effectiveness of the modulator in the analysis of a totally different sample-type.

The objective of the present research is directed towards the optimized use of a 50microm ID secondary column, in a comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GCxGC-qMS) system. The analytical aim was achieved by exploiting a split-flow GCxGC approach, and a rapid-scanning qMS instrument. The stationary phase combination consisted of an apolar (silphenylene polymer) 30mx0.25mm ID column, linked by means of a Y-union, to an MS-connected 1mx0.05mm ID polar one [poly(ethyleneglycol)], and to a 0.20mx0.05mm ID uncoated capillary segment; the latter was connected to a manually operated split-valve. It will be herein demonstrated that the split-flow GCxGC approach, successfully employed in previous H(2)-based, flame ionization detection experiments, provides equally satisfactory results using mass spectrometric detection and helium as carrier gas. An optimized split-flow GCxGC-qMS method was developed and exploited for the analysis of a perfume sample. The results attained were compared with those observed using the same analytical column combination, but with no flow-splitting. It was found that it is not convenient to employ a 50microm ID secondary column in a conventional GCxGC-MS instrument. On the contrary, the use a 50microm ID secondary column, in a split-flow, twin-oven system, provided a good performance. A recently developed comprehensive chromatography software was used for data processing.

A rapid extraction method involving microwave assisted extraction (MAE), followed by sample clean-up on a silica cartridge, reversed-phase high performance liquid chromatography (RP-HPLC) and spectrofluorimetric detection, was optimised for polycyclic aromatic hydrocarbon (PAH) determination in smoked meat. Compared to solvent extraction assisted by sonication, MAE, carried out with n-hexane on 2g of lyophilised sample at 115°C for 15min, allowed to obtain better extraction efficiencies. Limits of quantification (LOQ, s/n=10) lower than 0.2μg/kg wet weight were found for all PAHs, except for Fl (0.3μg/kg), P (0.6μg/kg) and IP (0.4μg/kg). The optimised procedure, that presented good analytical performances (with recoveries ranging from 77% to 103%, and precision within 10% for most of the PAHs), was applied to determine PAH content in different smoked meat products from the Italian market.

A solid-phase microextraction method coupled with comprehensive gas chromatography and time-of-flight mass spectrometry for the determination of polycyclic aromatic hydrocarbons in vegetable oils has recently been reported. The present paper tested the possibility to use the solid-phase microextraction method coupled with one-dimensional gas chromatography-mass spectrometry of the only benzo[a]pyrene. Furthermore, an in-house validation for benzo[a]pyrene, used as a marker, as requested by the European regulation no. 208/2005, was carried out. Statistical tests were performed to elaborate the data. Linearity was satisfactory (r(2)=0.999), between about 0.5 and 15 microg/kg. Detection limit and quantification limit were 0.17 and 0.46 microg/kg, respectively. In-day and inter-day repeatability were less than 6% in both cases.

Simple sample preparation procedures involving sonication and solid phase extraction (SPE), followed by reversed-phase high performance liquid chromatography (HPLC) and spectrofluorometric detection, were used to analyse polycyclic aromatic hydrocarbons (PAHs) in soil and olives collected in areas contaminated with creosote-treated railway ties. Very high PAH contents (with amounts ranging from 114.7 to 2157.2 and from 167.3 to 3121.8 μg kg− 1 dry weight for total light PAHs and total heavy PAHs, respectively) were found in soil sampled up to 1 m from the source of contamination. The PAH load decreased rapidly with the distance from the railway ties. High amounts of light PAHs, up to 6359.9 μg kg− 1, were also found in oil extracted from olives collected in a rural area where old railway ties were stored. No appreciable transfer of heavy PAHs and benzo[a]pyrene was observed in oil samples.