Occurrence of Fusarium mycotoxins and their dietary intake through beer consumption by the European population

Abstract Since cereals are raw materials for production of beer and beer-based drinks, the occurrence mycotoxins in 154 beer samples was topic of investigation in this study. The analyses were conducted using QuEChERS extraction and gas chromatography–tandem mass spectrometry determination. The analytical method showed recoveries for vast majority of analytes ranged from 70% to 110%, relative standard deviations lower than 15% and limits of detection from 0.05 to 8 μg/L. A significant incidence of HT-2 toxin and deoxynivalenol (DON) were found in 9.1% and 59.7% of total samples, respectively. The exposure of European population to mycotoxins through beer consumption was assessed. No toxicol…

Chemical Composition, In Vitro Bioaccessibility and Antioxidant Activity of Polyphenolic Compounds from Nutraceutical Fennel Waste Extract

Fennel (Foeniculum vulgare Mill.) waste contains a broad range of bioactive molecules, including polyphenols, which have poor bioaccessibility during gastrointestinal digestion. This work aimed to investigate the bioaccessibility of total phenolic compounds and the antioxidant capacity during simulated gastrointestinal digestion using two nutraceutical formulations based on non-acid-resistant (NAR) and acid-resistant (AR) capsules containing aqueous-based extracts from fennel waste. Moreover, to obtain a comprehensive investigation of the polyphenolic constituents of the fennel waste extract, a high-resolution mass spectrometry (Q-Orbitrap) analysis was performed. Notably, chlorogenic acids…

Determination of indoor air quality of a phytosanitary plant.

A new methodology has been developed to determine volatile organic compounds (VOCs) and pesticides in ambient air using membrane based devices as passive samplers. Pesticides were determined by gas chromatography with mass spectrometry detection (GC-MS) after their microwave-assisted extraction (MAE) from the passive sampler and the required clean-up. On the other hand, VOCs were also caught with the same samplers and directly determined by head space (HS) coupled to GC-MS. The use of samplers filled with florisil and activated carbon allows us to catch with a simple device both, VOCs and pesticides, with a high vapor pressure. Results obtained in the deployment of samplers in different sit…

Development of an UHPLC-Q-Orbitrap HRMS method for simultaneous determination of mycotoxins and isoflavones in soy-based burgers

Abstract Soy-based burgers, an option of meatless hamburger-style, are basically made with soy protein, wholegrains and veggies. However, some ingredients, such as cereals and soybean, are particularly susceptible to fungal contamination. Therefore, a fast and simple procedure for the simultaneous determination of isoflavones (n=12) and mycotoxins (n=21) in soy-based burgers was developed throughout an acetonitrile-based extraction and UHPLC-Q-Exactive Orbitrap HRMS determination for the first time. The procedure was properly validated in terms of linearity, accuracy (recovery range from 78 to 108%) and precision (RSD

Identification and Quantification of Enniatins and Beauvericin in Animal Feeds and Their Ingredients by LC-QTRAP/MS/MS

Emerging fusariotoxins, mainly enniatins (ENNs) and beauvericin (BEA), are secondary toxic metabolites produced by Fusarium spp. and are widely distributed contaminants of cereals and by-products. Mycotoxin contamination in these products supposes an important risk to feed supply security in the feed industry due to the common use of cereals in feed formulations. Hence, continuous monitoring of both raw materials and feed mixtures is highly recommended as stated by sanitary authorities. Therefore, an analytical procedure based on liquid chromatography tandem mass spectrometry and an acetonitrile-based extraction followed by a d-SPE (QuEChERS) step for the simultaneous determination of emerg…

Mouse tissue distribution and persistence of the food-born fusariotoxins Enniatin B and Beauvericin

The fusariotoxins Enniatin B (Enn B) and Beauvericin (Bea) have recently aroused interest as food contaminants and as potential anticancer drugs. However, limited data are available about their toxic profile. Aim of this study was to investigate their pharmacological behavior in vivo and their persistence in mice. Therefore, liquid chromatography tandem mass spectrometry (LC-MS/MS) was used to analyze the distribution of Enn B and Bea in selected tissue samples and biological fluids originating from mice treated intraperitoneally with these cyclohexadepsipeptides. Overall, no toxicological signs during life time or pathological changes were observed. Moreover, both fusariotoxins were found …

A preliminary study in Wistar rats with enniatin : A contaminated feed

A 28-day repeated dose preliminary assay, using enniatin A naturally contaminated feed through microbial fermentation by a Fusarium tricinctum strain, was carried out employing two months-old female Wistar rats as in vivo experimental model. In order to simulate a physiological test of a toxic compound naturally produced by fungi, five treated animals were fed during twenty-eight days with fermented feed. As control group, five rats were fed with standard feed. At the 28th day, blood samples were collected for biochemical analysis and the gastrointestinal tract, liver and kidneys were removed from each rat for enniatin A detection and quantitation. Digesta were collected from stomach, duode…

Transfer of Fusarium mycotoxins from malt to boiled wort

Malting was simulated using two different batches of barley as raw material: a naturally contaminated batch and laboratory inoculated (with a deoxynivalenol (DON) and zearalenone (ZEA) producing Fusarium graminearum strain) one. Up to three contamination levels were prepared, every process being carried out in triplicate. A significant washout effect on DON was observed by the end of the first water phase (between 22.4 and 34 % reduction) with an even more pronounced reduction (up to 75 % decrease) by the end of the steeping process. ZEA content remained almost unchanged (no significant difference between the initial and the final concentration). Germination was characterized by an increase…

Analysis of Phenolic Compounds in Commercial Cannabis sativa L. Inflorescences Using UHPLC-Q-Orbitrap HRMS

Industrial hemp (Cannabis sativa L. Family Cannabaceae) contains a vast number of bioactive relevant compounds, namely polyphenols including flavonoids, phenolic acids, phenol amides, and lignanamides, well known for their therapeutic properties. Nowadays, many polyphenols-containing products made of herbal extracts are marketed, claiming to exert health-promoting effects. In this context, industrial hemp inflorescence may represent an innovative source of bioactive compounds to be used in nutraceutical formulations. The aim of this work was to provide a comprehensive analysis of the polyphenolic fraction contained in polar extracts of four different commercial cultivars (Kompoti, Tiborszal…

Biological activity and toxicity of plant nutraceuticals: an overview

Plant nutraceuticals have currently been receiving international attention due to their potentially health-promoting effects when consumed as part of a varied diet, including antioxidant, anti-inflammatory, and anti-proliferative properties. These beneficial effects have been attributed to the presence of bioactive compounds naturally occurring in food or produced de novo through metabolic pathways. However, taken into account that nutraceuticals could be concentrated forms of the food or plants, it is probable to find undesirable substances utilized in crop protection, such as pesticides, and other contaminants (e.g. mycotoxins), which could be concentrated during the extraction process. H…

Interactions between T-2 toxin and its metabolites in HepG2 cells and in silico approach

Abstract The T-2 toxin (T-2) is commonly metabolized to HT-2 toxin (HT-2), Neosolaniol (NEO), T2-triol and T2-tetraol and they can modify the toxicity of T-2. In this study, T-2 and its modified forms were evaluated by in vitro and in silico methods. The in vitro cytotoxicity individually was evaluated by MTT and Total Protein Content (PC) assays in human hepatocarcinoma (HepG2) cells. The order of IC50 was T-2 tetraol > T-2 triol > NEO > T-2 = HT-2. The T-2 and HT-2 evidenced the highest cytotoxic effect in HepG2 cells individually. No differences were observed in binary combinations tested and the two mycotoxins in the mixture tested individually. The T-2+HT-2 combination showed the highe…

Cytoprotective Effects of Fish Protein Hydrolysates against H2O2-Induced Oxidative Stress and Mycotoxins in Caco-2/TC7 Cells

Many studies report the potent antioxidant capacity for fish protein hydrolysates, including radical scavenging activity and inhibition ability on lipid peroxidation (LPO). In this study, the in vitro cytotoxicity of protein hydrolysates from different salmon, mackerel, and herring side streams fractions was evaluated in the concentration range from 1 to 1:32 dilution, using cloned human colon adenocarcinoma cells TC7 (Caco-2/TC7) by MTT and PT assays. The protein hydrolysates’ antioxidant capacity and oxidative stress effects were evaluated by LPO and reactive oxygen species (ROS) generation, respectively. The antioxidant capacity for pure and bioavailable hydrolysate fraction was also eva…

T-2 toxin and its metabolites: Characterization, cytotoxic mechanisms and adaptive cellular response in human hepatocarcinoma (HepG2) cells

Abstract The T-2 toxin (T-2) is a type A trichothecene produced by Fusarium species, and the most cytotoxic mycotoxin of the group. A study was made to determine T-2 cytotoxicity in human hepatocarcinoma (HepG2) cells; evaluate whether there is an adaptive response of HepG2 cells exposed to low concentrations of T-2; identify the T-2 metabolites by LC-Q-TOF MS; and determine whether T-2 disrupts cell proliferation in HepG2 cells. The IC50 values obtained ranged from 61.9 ± 2.4 nM to 70.7 ± 7.4 nM. No adaptive response was observed. There was no evidence of extra- or intracellular accumulation of T-2 after 24 h of exposure as determined by LC-Q-TOF MS. However, some T-2 metabolites such as H…

Colon Bioaccessibility under In Vitro Gastrointestinal Digestion of Different Coffee Brews Chemically Profiled through UHPLC-Q-Orbitrap HRMS

Coffee represents one of the most traditionally consumed beverages worldwide, containing a broad range of human health&ndash

Deoxynivalenol contamination in cereal-based foodstuffs from Spain: Systematic review and meta-analysis approach for exposure assessment

Abstract The presence of deoxynivalenol (DON) has been repeatedly detected in cereal-based products collected from Spanish markets over the last years. Hence, the aim of this study was to conduct a systematic review and meta-analysis of the concentration and prevalence of DON in cereals and cereal-based products from Spanish markets intended for human consumption, in order to integrate the available data. Then, an exposure assessment was performed based on national consumption data. Results revealed a strong impact of DON in breakfast cereals (pooled concentration = 105.34 ng/g; pooled prevalence = 58%) and bread and derived products (pooled concentration = 95.17 ng/g; pooled prevalence = 6…

Development of microextraction techniques in combination with GC-MS/MS for the determination of mycotoxins and metabolites in human urine.

Simple and highly efficient sample preparation procedures, namely, dispersive liquid–liquid microextraction and salting-out liquid–liquid extraction for the analysis of ten Fusarium mycotoxins and metabolites in human urine were compared. Various parameters affecting extraction efficiency were carefully evaluated. Under optimal extraction conditions, salting-out liquid–liquid extraction showed a better accuracy (84–96%) and precision (<14%) than dispersive liquid–liquid microextraction. Hence, a multibiomarker method based on salting-out liquid–liquid extraction followed by gas chromatography with tandem mass spectrometry was proposed. Satisfactory results in terms of validation were achiev…

Target Quantification and Semi-Target Screening of Undesirable Substances in Pear Juices Using Ultra-High-Performance Liquid Chromatography-Quadrupole Orbitrap Mass Spectrometry.

Fruit juices are common products in modern diets due to the supply of vegetal nutrients combined with its tastiness. Nevertheless, potential contaminants, such as mycotoxins and pesticides, can be present in commercial products due to a potential carry-over. Therefore, the aim of this study was to investigate for the first time the presence of 14 Fusarium mycotoxins using a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction followed by an ultra-high-performance liquid chromatography-quadrupole Orbitrap high-resolution mass spectrometry in 21 pear juice samples from Italian markets. Up to nine different mycotoxins were detected, particularly an extensive presence of …

A survey of trichothecenes, zearalenone and patulin in milled grain-based products using GC-MS/MS.

An analytical protocol based on QuEChERS and gas chromatography-tandem mass spectrometry (GC-MS/MS) was successfully applied for the determination of trichothecenes, patulin and zearalenone in 182 milled grain-based samples. The analytical method was validated following the SANCO 1495/2011 document. LOQs were lower than 10μgkg(-1) for the selected mycotoxins. Recoveries of fortified cereals ranged between 76-108% and 77-114% at 20 and 80μgkg(-1), respectively, with relative standard deviation lower than 9%. More than 60% of the samples analysed showed deoxynivalenol contamination, followed by HT-2 toxin and nivalenol with frequencies of 12.1% and 10.4%, respectively. Co-occurrence of mycoto…

Fast analysis of polyphenols and alkaloids in cocoa-based products by ultra-high performance liquid chromatography and Orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap-MS/MS).

The cocoa varieties Criollo, Forastero and Trinitario, which have different organoleptic properties, quite often are mixed together in cocoa-based products. The objective of this work was to develop a rapid method for the simultaneous determination of polyphenols (n = 35) and alkaloids (n = 2) in cocoa-based products by using the high throughput advantages provided by the Q Exactive Hybrid Quadrupole-Orbitrap Mass Spectrometer (FIRMS). The proposed procedure was optimized and validated in terms of selectivity and specificity (mass accuracy 0.990), accuracy (recovery range from 89.1 to 112.4%) and precision (relative standard deviation < 10%). The method was applied to 80 cocoa-based samples…

Monitoring Alternaria mycotoxins and pesticide residues in tomato by dispersive liquid–liquid microextraction coupled to gas chromatography–tandem mass spectrometry

Quantitative determination of trichothecenes in breadsticks by gas chromatography-triple quadrupole tandem mass spectrometry.

Breadsticks are pencil-sized sticks of dry bread widely consumed as a pre-meal appetiser. They are basically wheat-based snacks, which makes them a good matrix to evaluate mycotoxin contamination, since wheat is very susceptible to fungal attack. In this sense, the fast, selective and sensitive gas chromatography-triple quadrupole tandem mass spectrometry (GCQqQ- MS/MS) method proposed here allows simultaneous determination of deoxynivalenol (DON), 3-acetyldeoxynivalenol, fusarenon-X, diacetoxyscirpenol, nivalenol, neosolaniol, HT-2 and T-2 toxin in breadsticks after QuEChERS extraction and clean-up. The performance of the method was assessed with respect to European Commission Regulations …

Determination of trichothecenes in chicken liver using gas chromatography coupled with triple-quadrupole mass spectrometry

Abstract Chicken meat and edible offal are included in a wide number of preparations in the worldwide cuisine. Among the offal, the liver is one of the most consumed in some countries like Egypt since it is rich in proteins and is an economical source of many essential nutrients for humans. Mycotoxins, secondary toxic metabolites produced by fungi, have the potential to enter human food chain not only with cereal consumption but also through edible tissues from animals fed with mycotoxin-contaminated feed. Accordingly, a rapid method for the determination of eight trichothecenes in chicken liver was developed based on a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction an…

Determination of mycotoxins in bee pollen by gas chromatography-tandem mass spectrometry.

Bee pollen, promoted as a natural food supplement, is consumed increasingly by people to maintain a healthy diet. Depending on environmental conditions, pollen can also be an optimum medium for growth of molds such as Fusarium and Penicillium . A quick, easy, cheap, rapid, and safe (QuEChERS) extraction procedure followed by a gas chromatography-tandem mass spectrometry (GC-MS/MS) determination of eight selected Fusarium toxins in bee pollen was developed and optimized. Recovery studies at 20, 80, and 1000 μg/kg showed values between 73 and 95% with relative standard deviations (RSDs) of15% for all studied mycotoxins. Limits of quantitation (LOQ) ranged from 1 to 4 μg/kg. The proposed metho…

The Natural Fungal Metabolite Beauvericin Exerts Anticancer Activity In Vivo: A Pre-Clinical Pilot Study

Recently, in vitro anti-cancer properties of beauvericin, a fungal metabolite were shown in various cancer cell lines. In this study, we assessed the specificity of this effect by comparing beauvericin cytotoxicity in malignant versus non-malignant cells. Moreover, we tested in vivo anticancer effects of beauvericin by treating BALB/c and CB-17/SCID mice bearing murine CT-26 or human KB-3-1-grafted tumors, respectively. Tumor size and weight were measured and histological sections were evaluated by Ki-67 and H/E staining as well as TdT-mediated-dUTP-nick-end (TUNEL) labeling. Beauvericin levels were determined in various tissues and body fluids by LC-MS/MS. In addition to a more pronounced …

Development and Validation of a LC-ESI-MS/MS Method for the Determination of Alternaria Toxins Alternariol, Alternariol Methyl-Ether and Tentoxin in Tomato and Tomato-Based Products

Alternaria species are capable of producing several secondary toxic metabolites in infected plants and in agricultural commodities, which play important roles in food safety. Alternaria alternata turn out to be the most frequent fungal species invading tomatoes. Alternariol (AOH), alternariol monomethyl ether (AME), and tentoxin (TEN) are some of the main Alternaria mycotoxins that can be found as contaminants in food. In this work, an analytical method based on liquid chromatography (LC) tandem mass spectrometry (MS/MS) detection for the simultaneous quantification of AOH, AME, and TEN in tomato and tomato-based products was developed. Mycotoxin analysis was performed by dispersive liquid-…

Development of a GC–MS/MS strategy to determine 15 mycotoxins and metabolites in human urine

The widespread mycotoxins contamination of food commodities has made the monitoring of their levels essential. To overcome the disadvantages of the indirect approach by food analysis, detection of mycotoxin as biomarkers in urine provides a useful and specific data for exposure assessment to these food contaminants. In this work, a sensitive, rapid and accurate method based on gas chromatography-tandem mass spectrometry procedure to determine 15 mycotoxins and metabolites in human urine was optimized and validated taking into consideration the guidelines specified in Commission Decision 2002/657/EC and 401/2006/EC. A salting-out assisted acetonitrile-based extraction was used for sample pre…

Biomonitoring of Enniatin B1 and Its Phase I Metabolites in Human Urine: First Large-Scale Study

Enniatins (Enns) are mycotoxins produced by Fusarium spp. which are a fungus widely spread throughout cereals and cereal-based products. Among all the identified enniatins, Enn B1 stands as one of the most prevalent analogues in cereals in Europe. Hence, the aim of this study was to evaluate for the first time the presence of Enn B1 and its phase I metabolites in 300 human urine samples using an ultrahigh-performance liquid chromatography high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) methodology. Enn B1 was detected in 94.3% of samples ranging from 0.007 to 0.429 ng/mL (mean value: 0.065 ng/mL). In accordance with previous in vitro and in vivo analysis, hydroxylated metabolites …

Target analysis and retrospective screening of mycotoxins and pharmacologically active substances in milk using an ultra-high-performance liquid chromatography/high-resolution mass spectrometry approach.

Milk is a nutritious food suitable for infants and adults, and it plays an important role in the human diet. However, it may also be a vehicle for food contaminants. In this report, we developed a method using ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap HRMS; Thermo Fisher Scientific, Waltham, MA) for simultaneous identification of target pharmacologically active substances and mycotoxins in milk. We also used the Q-Orbitrap operating in full scan mode to identify other possible drugs and microbial metabolites that occurred in samples. Fifty-six commercially available milk samples from the Italian market were analyze…

Citrinin Dietary Exposure Assessment Approach through Human Biomonitoring High-Resolution Mass Spectrometry-Based Data.

Citrinin (CIT) is a scarcely studied mycotoxin within foodstuffs, so the biomonitoring of this toxin and its metabolite dihydrocitrinone (DH-CIT) in biological samples represents the main alternative to estimate the exposure. Hence, this study aimed to evaluate the presence of CIT and DH-CIT in 300 urine samples from Italian individuals in order to assess the exposure. Quantification was performed through an ultrahigh-performance liquid chromatography high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS)-based methodology. CIT was quantified in 47% of samples (n = 300) up to 4.0 ng/mg Crea (mean = 0.29 ng/mg Crea), whereas DH-CIT was quantified in 21% of samples up to 2.5 ng/mg Crea (me…

Exposure estimates to Fusarium mycotoxins through cereals intake.

Abstract Mycotoxins are harmful substances produced by fungi in several commodities with a widespread presence in foodstuffs. Human exposure to mycotoxins occurs mainly by contaminated food. The quantitation of mycotoxins in cereal-based food, highly consumed by different age population, is of concern. In this survey, 159 cereal-based samples classified as wheat, maize and rice-based, have been evaluated for the occurrence of patulin, deoxynivalenol, 3-acetyl-deoxynivalenol, fusarenon-X, diacetoxyscirpenol, nivalenol, neosolaniol, HT-2, T-2 and zearalenone by gas chromatography–tandem mass spectrometry. Intakes were calculated for average consumers among adults, children and infants and com…

Target Analysis and Retrospective Screening of Multiple Mycotoxins in Pet Food Using UHPLC-Q-Orbitrap HRMS

A comprehensive strategy combining a quantitative method for 28 mycotoxins and a post-target screening for other 245 fungal and bacterial metabolites in dry pet food samples were developed using an acetonitrile-based extraction and an ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) method. The proposed method showed satisfactory validation results according to Commission Decision 2002/657/EC. Average recoveries from 72 to 108% were obtained for all studied mycotoxins, and the intra-/inter-day precision were below 9 and 14%, respectively. Results showed mycotoxin contamination in 99% of pet food samples (n = 89) at concentratio…

Chemical Composition of Green Pea (Pisum sativum L.) Pods Extracts and Their Potential Exploitation as Ingredients in Nutraceutical Formulations

Agro-industrial wastes contain a large number of important active compounds which can justify their use as innovative ingredients in nutraceutical products. This study aimed to provide a complete analysis of active molecules, namely (poly)phenols in pea pods water-based extracts, through a UHPLC-Q-Orbitrap HRMS methodology. Data showed that 5-caffeoylquinic acid, epicatechin, and hesperidin were the most relevant (poly)phenols found in the assayed extracts, with a mean value of 59.87, 29.46, and 19.94 mg/100 g, respectively. Furthermore, changes in antioxidant capacity and bioaccessibility of total phenolic compounds (TPC) after the simulated gastrointestinal (GI) process were performed usi…

Occurrence and exposure assessment of mycotoxins in ready-to-eat tree nut products through ultra-high performance liquid chromatography coupled with high resolution q-orbitrap mass spectrometry

Tree nuts have become popular snacks due to their attributed benefits in the health state. Nevertheless, their susceptibility to fungal contamination lead to the occurrence of potentially dangerous mycotoxins. Hence, the aim of this work was to evaluate the presence of mycotoxins in ready-to-eat almonds, walnuts, and pistachios from Italian markets. The most relevant mycotoxin found in almonds was &alpha;-zearalanol in 18% of samples (n = 17) ranging from 3.70 to 4.54 &micro;g/kg. Walnut samples showed frequent contamination with alternariol, present in 53% of samples (n = 22) at levels from 0.29 to 1.65 &micro;g/kg. Pistachios (n = 15) were the most contaminated commodity, with &beta;-zear…

Multi-mycotoxin analysis in wheat semolina using an acetonitrile-based extraction procedure and gas chromatography–tandem mass spectrometry

A new analytical method for the rapid and simultaneous determination of ten mycotoxins including patulin, zearalenone and eight trichothecenes (nivalenol, fusarenon-X, diacetoxyscirpenol, 3-acetyl-deoxynivalenol, neosolaniol, deoxynivalenol, T-2 and HT-2) in wheat semolina has been developed and optimized. Sample extraction and purification were performed with a modified QuEChERS-based (acronym of Quick, Easy, Cheap, Effective, Rugged and Safe) procedure and determined by gas chromatography (GC) coupled to triple quadrupole instrument (QqQ). This is the first paper on the application of GC-QqQ-MS/MS to analysis of mycotoxins. Careful optimization of the gas chromatography-tandem mass spectr…

Mycotoxin Occurrence and Risk Assessment in Gluten-Free Pasta through UHPLC-Q-Exactive Orbitrap MS

Celiac disease (CD) is a genetic-based autoimmune disorder which is characterized by inflammation in the small intestinal mucosa due to the intolerance to gluten. Celiac people should consume products without gluten, which are elaborated mainly with maize or other cereals. Contamination of cereals with mycotoxins, such as fumonisins (FBs) and aflatoxins (AFs) is frequently reported worldwide. Therefore, food ingestion is the main source of mycotoxin exposure. A new analytical method was developed and validated for simultaneous analysis of 21 mycotoxins in gluten-free pasta, commonly consumed by celiac population as an alternative to conventional pasta. Ultrahigh-performance liquid chromatog…

Preliminary Estimation of Deoxynivalenol Excretion through a 24 h Pilot Study

A duplicate diet study was designed to explore the occurrence of 15 Fusarium mycotoxins in the 24 h-diet consumed by one volunteer as well as the levels of mycotoxins in his 24 h-collected urine. The employed methodology involved solvent extraction at high ionic strength followed by dispersive solid phase extraction and gas chromatography determination coupled to mass spectrometry in tandem. Satisfactory results in method performance were achieved. The method"s accuracy was in a range of 68%108%, with intra-day relative standard deviation and inter-day relative standard deviation lower than 12% and 15%, respectively. The limits of quantitation ranged from 0.1 to 8 μg/Kg. The matrix effect w…

Ultra-High-Performance Liquid Chromatography Coupled with Quadrupole Orbitrap High-Resolution Mass Spectrometry for Multi-Residue Analysis of Mycotoxins and Pesticides in Botanical Nutraceuticals

Cannabidiol (CBD) food supplements made of Cannabis sativa L. extracts have quickly become popular products due to their health-promoting effects. However, potential contaminants, such as mycotoxins and pesticides, can be coextracted during the manufacturing process and placed into the final product. Accordingly, a novel methodology using ultra-high-performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was developed to quantify 16 mycotoxins produced by major C. sativa fungi, followed by a post-target screening of 283 pesticides based on a comprehensive spectral library. The validated procedure was applied to ten CBD-bas…

Colon bioaccessibility under in vitro gastrointestinal digestion of a red cabbage extract chemically profiled through UHPLC‐Q‐Orbitrap HRMS

Red cabbage is a native vegetable of the Mediterranean region that represents one of the major sources of anthocyanins. The aim of this research is to evaluate the antioxidant capability and total polyphenol content (TPC) of a red cabbage extract and to compare acquired data with those from the same extract encapsulated in an acid-resistant capsule. The extract, which was qualitatively and quantitatively profiled by UHPLC-Q-Orbitrap HRMS analysis, contained a high content of anthocyanins and phenolic acids, whereas non-anthocyanin flavonoids were the less abundant compounds. An in vitro gastrointestinal digestion system was utilized to follow the extract&rsquo

Urinary levels of enniatin B and its phase I metabolites: First human pilot biomonitoring study

Abstract Enniatins (Enns) are mycotoxins produced by Fusarium spp. and are widely distributed contaminants of cereals and derivate products. Among the different identified enniatins, Enn B is the most relevant analogue in cereals in Europe. Therefore, the aim of this study was to investigate for the first time the occurrence of Enn B and Enn B phase I metabolites in 300 human urine samples throughout an ultrahigh-performance liquid chromatography-high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) methodology. Three different sample preparation procedures were evaluated and salting-out liquid-liquid extraction showed satisfactory validation results. Enn B was quantified in 83.7% of sa…

Exposure assessment approach through mycotoxin/creatinine ratio evaluation in urine by GC–MS/MS

Abstract In this pilot survey human urine samples were analyzed for presence of 15 mycotoxins and some of their metabolites using a novel urinary multi-mycotoxin GC–MS/MS method following salting-out liquid–liquid extraction. Fifty-four urine samples from children and adults residents in Valencia were analyzed for presence of urinary mycotoxin and expressed in gram of creatinine. Three out of 15 mycotoxins were detected namely, HT-2 toxin, nivalenol and deoxynivalenol (DON). 37 samples showed quantifiable values of mycotoxins. Co-occurrence of these contaminants was also observed in 20.4% of assayed samples. DON was the most frequently detected mycotoxin (68.5%) with mean levels of 23.3 μg/…

Multi-mycotoxin occurrence in feed, metabolism and carry-over to animal-derived food products: A review

The world requests for raw materials used in animal feed has been steadily rising in the last years driven by higher demands for livestock production. Mycotoxins are frequent toxic metabolites present in these raw materials. The exposure of farm animals to mycotoxins could result in undesirable residues in animal-derived food products. Thus, the potential ingestion of edible animal products (milk, meat and fish) contaminated with mycotoxins constitutes a public health concern, since they enter the food chain and may cause adverse effects upon human health. The present review summarizes the state-of-the-art on the occurrence of mycotoxins in feed, their metabolism and carry-over into animal …