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The knowledge of chloropropanediols (MCPD) fatty acid esters formation pathways is an important condition for these processing contaminants mitigation. This study aimed to assess the potential of a group of lipophilic environmental contaminants, polychlorinated alkanes, commonly known as chlorinated paraffins (CPs), to contribute to the formation of MCPD esters. Laboratory-scale model systems representing vegetable oils contaminated with both a technical mixture of short-chained CPs and individual short-chained CPs were designed and subjected to heat treatment (230 °C, 2 h) to simulate the deacidification and deodorisation processes. A substantial increase in MCPD content (up to 3.4 times the control levels) was observed in systems spiked with a technical mixture. MCPD formation seems to correlate very well with the concentration of CPs in these systems. Based on the generated data, we can conclude that the processing of vegetable oils contaminated with CPs might contribute to elevated concentrations of MCPD., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Malting and brewing have previously been demonstrated to be risky procedures in terms of mycotoxins contamination. The goal of the study was to describe the fate of less investigated Fusarium and Alternaria mycotoxins, together with their conjugates, during these processes. The Pilsner malt producing process, together with double-mash brewing, were performed in a pilot-scale malting and brewery plants to simulate production of lager - the most popular type of central European beer. In addition, changes in temperature during barley germination were investigated to assess the influence of this critical step. QuEChERS-like extraction followed by UHPLC-HRMS/MS were utilized to quantify the mass balance of 13 mycotoxins and four of their conjugates. The results confirmed germination as the most determining malting step, followed by mashing of malt during brewing. Occurrence of type A trichothecenes, Alternaria mycotoxins and their conjugates in the final beer product indicates the need to take mitigation measures., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Use of 'green biomass' of the grapevine is gradually extending into the food industry. The aim of our study was to demonstrate the potential of metabolomic fingerprinting for characterization of grapevine leaves and canes. Our method comprises successive aqueous-methanolic extractions, followed by U-HPLC-HRMS/MS. For data processing, PCA and (O)PLS-DA methods were utilized, and mathematical models were validated. We showed that from all factors investigated, harvesting season explained most of the variability between samples, followed by locality combined with farming system. The identified statistically significant metabolites for harvesting season models mostly represented the groups of fatty acids, fatty phenols, (lyso)phospholipids, flavonoids and organic acids. For models of localities with different farming systems, majority of identified metabolites significant for organic farming belonged to groups of fatty acids and their derivatives, terpenoids, sterols, and fat soluble vitamins, whereas for conventional farming, the only identified significant metabolites were the pesticide residues., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

The aim of this study was to develop methods for the determination of short- and medium-chain chlorinated paraffins (SCCPs; MCCPs) in vegetable oils and fish employing gas chromatography coupled with high-resolution mass spectrometry because of a lack of information on the presence of chlorinated paraffins in food consumed in Europe. For isolation of CPs from fish, an ethyl acetate extraction followed by a clean-up of the extract by gel permeation chromatography was performed. The same purification step was used for the isolation of CPs from the vegetable oils. The concentration range for SCCPs was <10-389 ng/g lipid weight (lw, mean 36 ng/g lw for the oils and 28 ng/g lw for the fish) and that for MCCPs was <20-543 ng/g lw (mean 55 ng/g lw for the oils and 59 ng/g lw for the fish). There was found a high variability in concentrations of CPs influenced by area of origin., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

The influence of dough composition on acrylamide, 3-monochloropropane-1,2-diol (3-MCPD) esters, and glycidyl esters (GE) formation during bread toasting was investigated. The doughs differed in added amounts of soy lecithin, salt, and reducing agents (l-cysteine and glutathione). The toasting of bread for 2.5 min considerably enhanced the formation of acrylamide and 3-MCPD esters. The addition of lecithin (1%, w/w) resulted in four times higher content of 3-MCPD esters in toasted bread slices. No distinct relationship between dough composition and GE formation in untoasted and toasted bread was found. The addition of reducing agents (0.05%, w/w) mitigated during toasting not only the formation of 3-MCPD esters (more than six times) but also the extent of Maillard reaction that resulted in three times lower amounts of acrylamide and predominant formation of alcohol-like compounds. Toasted bread without reducing agents contained typical Maillard reaction compounds such as aldehydes, alkyl pyrazines, and derivatives of furan., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Due to unique phytochemicals contained, Vaccinum berries are known to have a number of positive health effects. In this context, lingonberries (Vaccinium vitis-idaea) are considered to be the most effective, thus finding many uses. Recently, fraud suspicion on lingonberries-based products has been reported, partial or even total replacement by less valued cranberries (Vaccinium macrocarpon) was found. In this study, metabolomic fingerprinting employing instrumental platform consisting of U-HPLC-HRMS/MS was investigated for discrimination between the two Vaccinum berries species. Methanolic extracts of 33 authentic samples from two harvest years were analyzed and chemometric evaluation was performed to identify significant marker compounds, their stability during drying process was assessed, too. The characteristic markers most contributing to berries classification were representatives of polyphenols and phospholipids. Peonidin 3-O-arabinoside and myricetin 3-O-glucoside, not occurring in lingonberries, enabled to discover the presence of cranberries in prepared admixtures down to 1% (w/w)., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Oregano, a widely used and popular herb, is particularly vulnerable to fraud. Less valued plants, adulterants that are often used for dilution, may introduce into this commodity additional contaminants such as pesticide residues. In this study, more than 400 pesticides were screened in a representative set of 42 genuine and 34 adulterated dried oregano samples collected from various locations across Europe. The results obtained by advanced mass spectrometry-based methods, showed, that some pesticide residues could be detected in virtually all tested samples, nevertheless, on average, higher contamination was found in the adulterated oregano samples. Increased incidence of insecticides such as cyfluthrin, permethrin and cyhalothrin was typical for these samples, moreover, pyriproxyfen was detected exclusively in adulterated samples. Thus, based on a critical assessment of pesticide profiles, suspected adulterated oregano samples can be selected for follow up authenticity testing., (Copyright © 2018 The Authors. Published by Elsevier Ltd.. All rights reserved.)

This work was designed as a proof of concept, to demonstrate the successful use of the comparison between theoretical and experimental collision cross section (CCS) values to support the identification of isomeric forms. To this purpose, thirteen mycotoxins were considered and analyzed using drift time ion mobility mass spectrometry. A good linear correlation (r 2  = 0.962) between theoretical and experimental CCS was found. The average ΔCCS was 3.2%, fully consistent with the acceptability threshold value commonly set at 5%. The agreement between theoretical and experimental CCS obtained for mycotoxin glucuronides suggested the potential of the CCS matching in supporting the annotation procedure., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

This research was focused on a critical assessment of vacuum frying as a technology enabling minimization of acrylamide formation in potato crisps and reducing undesirable chemical changes that occur in frying oil at high temperatures. The potato slices were fried in rapeseed oil under vacuum at 125°C and atmospheric pressure at 165°C. The experiments were performed on two potato varieties, Saturna and Impala. Vacuum frying reduced the formation of acrylamide by 98% and also other Maillard reaction products, specifically alkylpyrazines. Concurrently a lower extent of oxidative changes was observed in the frying oil, while 3-MCPD esters decreased fairly quickly during conventional frying. Sensory characteristics of the vacuum and conventionally fried potato crisps were evaluated by a 23-member panel. The majority of panellists preferred the flavour of 'conventional crisps', while only a few of them appreciated potato-like fresh flavour of 'vacuum crisps' and classified this product as 'tasty'., (Copyright © 2017. Published by Elsevier Ltd.)

In the present work the possibility of using an untargeted metabolomic strategy to discriminate between common and durum wheat lipidome for an authenticity purpose was explored. A first study was conducted by analyzing 52 samples from two durum and common wheat varieties. Afterwards, an extended and independent sample set (173 samples and five varieties) was used as a confirmatory study to verify the stability and consistency of the models obtained. Putatively identified markers were evaluated applying ROC curves resulting in individual marker AUC >90% both in preliminary and confirmatory study. In addition, digalactosyl diglyceride (DGDG) 36:4 was shown to be an effective marker differentiating between authentic durum wheat and its adulterated admixture down to 3% adulteration level, which is the maximum contamination level allowed by Italian legislation. The results demonstrated that untargeted lipidomics, in conjunction with chemometric tools has a significant potential for screening and detection of wheat fraud., (Copyright © 2017. Published by Elsevier Ltd.)

In order to explore the early detection of mycotoxins in wheat three standardized approaches (Fusarium disease severity, PCR assays for Fusarium spp. identification and mycotoxin quantification) and a novel untargeted metabolomics strategy were jointly assessed. In the first phase of this research, standardized approaches were able to quantify mycotoxins and identify Fusarium spp. Then, an UHPLC-QTOF metabolic fingerprinting method was developed to investigate plant-pathogen cross-talk. At the same time, chemometrics analysis demonstrated to be a powerful tool in order to distinguish low and strong infection levels. Combining these results, the cross-talk plant pathogen related to the early detection of mycotoxins was discovered. As a rapid response to fungal infection an overexpression of phosphatidic acids was discovered. By contrast, when the infection became stronger an increase of oxylipins and diacylglycerols was revealed., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Saffron is one of the oldest and most expensive spices, which is often target of fraudulent activities. In this research, a new strategy of saffron authentication based on metabolic fingerprinting was developed. In the first phase, a solid liquid extraction procedure was optimized, the main aim was to isolate as maximal representation of small molecules contained in saffron as possible. In the second step, a detection method based on liquid chromatography coupled with high-resolution mass spectrometry was developed. Initially, principal component analysis (PCA) revealed clear differences between saffron cultivated and packaged in Spain, protected designation of origin (PDO), and saffron packaged in Spain of unknown origin, labeled Spanish saffron. Afterwards, orthogonal partial least square discriminant analysis (OPLS-DA) was favorably used to discriminate between Spanish saffron. The tentative identification of markers showed glycerophospholipids and their oxidized lipids were significant markers according to their origin., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The objective of this study is the evaluation of the potential of high-throughput direct analysis in real time-high resolution mass spectrometry (DART-HRMS) fingerprinting and multivariate regression analysis in prediction of the extent of acrylamide formation in biscuit samples prepared by various recipes and baking conditions. Information-rich mass spectral fingerprints were obtained by analysis of biscuit extracts for preparation of which aqueous methanol was used. The principal component analysis (PCA) of the acquired data revealed an apparent clustering of samples according to the extent of heat-treatment applied during the baking of the biscuits. The regression model for prediction of acrylamide in biscuits was obtained by partial least square regression (PLSR) analysis of the data matrix representing combined positive and negative ionization mode fingerprints. The model provided a least root mean square error of cross validation (RMSECV) equal to an acrylamide concentration of 5.4 μg kg(-1) and standard error of prediction (SEP) of 14.8 μg kg(-1). The results obtained indicate that this strategy can be used to accurately predict the amounts of acrylamide formed during baking of biscuits. Such rapid estimation of acrylamide concentration can become a useful tool in evaluation of the effectivity of processes aiming at mitigation of this food processing contaminant. However, the robustness this approach with respect to variability in the chemical composition of ingredients used for preparation of biscuits should be tested further., (Copyright © 2014. Published by Elsevier Ltd.)

Transmission-mode direct analysis in real time ionization coupled with high resolution mass spectrometry (TM-DART-HRMS) was used to monitor chemical changes in various vegetable oils (olive, rapeseed, soybean and sunflower oil) during their thermally-induced oxidation. This novel instrumental approach enabled rapid fingerprinting of examined samples and detection of numerous sample components, such as triacylglycerols (TAGs), phytosterols, free fatty acids (FFA), and their respective oxidation products. Mass spectra obtained from DART were processed with the use of principal component analysis (PCA) in order to assess the compositional differences between heated and non-heated samples. Good correlation was observed between the normalized intensities of the pre-selected ion corresponding to mono-oxidized TAG and 'classic' criterion represented by the levels of TAG polymers determined by high performance-size exclusion chromatography with refractometric detection (HP-SEC-RID)., (Copyright © 2013. Published by Elsevier Ltd.)

Enniatins represent an emerging food safety issue because of their extensive incidence, documented in recent decades, in various small grain cereals. This study was concerned with the fate of these Fusarium mycotoxins within malting, brewing, milling and baking, when employed for the processing of contaminated barley and wheat. Besides enniatins A, A1, B and B1, also deoxynivalenol and its conjugated form (deoxynivalenol-3-glucoside) were determined in almost all tested cereal-based samples. Significant decline of enniatins occurred within all technologies, with the largest drop in their concentrations observed in the brewing process. While enniatins were not detectable in final beers, they were almost quantitatively transferred to spent grains, probably because of their limited water solubility. Regarding bread baking, levels of enniatins decreased down to 30% of their concentration in the initial flour used for baking. In this case, degradation at higher temperatures might be assumed., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

The co-occurrence of deoxynivalenol (DON) and deoxynivalenol-3-glucoside (DON-3-Glc) has been recently reported in malt and beer. In this study, the concentration changes were monitored within the brewing process of four beer brands: light, dark tap and two lagers, produced from ground malt mixtures differing in composition, and also mycotoxins content. A simple and rapid method employing DON-dedicated immunoaffinity columns (IAC) for the selective pre-concentration, followed by ultra-performance liquid chromatography coupled to a time-of-flight mass spectrometer (UPLC-TOFMS) system for the reliable quantification at (ultra)trace levels, was validated for all experimental matrices. The results document the key role of the malt contamination nature. While in the first monitoring period a significant increase of both DON and DON-3-Glc occurred (up to 250% and 450%, respectively), fairly different trends were observed when new malts were used for identical technological processing (in some beers a decrease of DON and only a small increase of DON-3-Glc occurred). Worth noticing, that the outcome of the brewing process was surprisingly reproducible for a particular malt mixture. In the final phase, a small monitoring study comparing Czech and Austrian alcohol-free and conventional beers was carried out., (Copyright © 2010 Elsevier Ltd. All rights reserved.)