Determination of several aminoglycoside and macrolide antibiotics in animal tissues by liquid chromatography-electrospray ionization-tandem mass spectrometry
Risk assessment associated to the intake of the emerging Fusarium mycotoxins BEA, ENs and FUS present in infant formula of Spanish origin
Abstract Forty-five samples of Spanish follow-up infant formula with different chemical compositions were analyzed determining the emerging Fusarium mycotoxins beauvericin (BEA), enniatins (ENs) (A, A 1 , B, B 1 ), and fusaproliferin (FUS). The samples were extracted three times with ethyl acetate using an Ultra-turrax homogenizer. Mycotoxins were identified and quantified using a liquid chromatography (LC) coupled to a diode array detector (DAD). Results showed that the percentage of the samples contaminated with ENs and FUS were 46.6 and 20.0% respectively, whereas all analyzed samples were free of BEA. The ENs A and B were detected only in one sample with 149.6 and 39.4 mg/kg respectivel…
Nuts and dried fruits: Natural occurrence of emerging Fusarium mycotoxins
Abstract The occurrence of enniatins (ENs) and beauvericin (BEA) in nuts, dried fruits and dates available in Valencia (Spain) was surveyed in this study. To do this, seventy-four samples of nuts, dried fruits and dates were analyzed for the determination of mycotoxin contamination. Mycotoxins were identified and quantified using an ultrasonic-C18 extraction and LC–MS/MS with a triple quadrupole (QqQ) mass analyzer. The frequencies of contamination of nuts, shell, dried fruits and dates were 50%, 80%, 35.7% and 83.3%, respectively. Enniatin A (ENA) was the most predominant EN found in nuts (45.2%) while ENB was the most common EN found in dates (58.3%). The analytical results of the shell s…
Multi-Mycotoxin Analysis in Durum Wheat Pasta by Liquid Chromatography Coupled to Quadrupole Orbitrap Mass Spectrometry.
A simple and rapid multi-mycotoxin method for the determination of 17 mycotoxins simultaneously is described in the present survey on durum and soft wheat pasta samples. Mycotoxins included in the study were those mainly reported in cereal samples: ochratoxin-A (OTA), aflatoxin B1 (AFB1), zearalenone (ZON), deoxynivalenol (DON), 3-and 15-acetyl-deoxynivalenol (3-AcDON and 15-AcDON), nivalenol (NIV), neosolaniol (NEO), fusarenon-X, (FUS-X), T-2 toxin (T-2) and HT-2 toxin (HT-2), fumonisin B1 and B2 (FB1 and FB2), and four emerging mycotoxins: three enniatins (ENA, ENA1, and ENB), and beauvericin (BEA). Twenty-nine samples were analyzed to provide an overview on…
Mitigation of enniatins in edible fish tissues by thermal processes and identification of degradation products.
Emerging mycotoxins, such as enniatins and beauvericin, are common contaminants in vegetal matrices, but recently, the occurrence of mycotoxins in foodstuffs from animal origin has been also reported as they can be present in edible tissues of animals fed with contaminated feedstuffs. Sea bass, sea bream, Atlantic salmon and rainbow trout from aquaculture analyzed in the present survey showed contamination by emerging Fusarium mycotoxins enniatins (ENs). ENs were extracted from raw and cooked fish with acetonitrile and analyzed by Liquid Chromatography coupled to Mass Spectrometry. In this study, the stability of ENs was evaluated during food processing by the application of different cooki…
High-performance liquid chromatographic determination of furfural compounds in infant formulas during full shelf-life
Abstract In order to evaluate the extent of the Maillard reaction in adapted and follow-up infant formulas (IF), a study was made of the evolution of furfural compound (2-furaldehyde, 5-hydroxymethyl-2-furfuraldehyde, 2-furylmethylketone and 5-methyl-2-furaldehyde) in these products, along with their relation to available lysine during the shelf-life period (two years at 20 and 37 °C). Total and free furfural contents were measured by RP-HPLC and UV detection, heating or not the sample in boiling water to free the furfurals bound to proteins and the furfurals formed from precursors. Only 2-furylmethylketone and 5-hydroxymethyl-2-furfuraldehyde were detected. Adapted and follow-up IF showed …
Comparative assessment of three extraction procedures for determination of emerging Fusarium mycotoxins in pasta by LC–MS/MS
Abstract A new rapid, sensitive, reproducible and reliable method was developed for the quantitative determination of enniatins A, A1, B and B1, beauvericin and fusaproliferin in dry and fresh pasta by liquid chromatography-triple quadrupole-tandem mass spectrometry. A comparative study of different rapid and economical extraction procedures was performed for the extraction of these mycotoxins in pasta. For this purpose, three different approaches were studied during the extraction step (Ultra-Turrax, ultrasonic bath and microwave). Optimal extraction conditions were reached using Ultra-Turrax with acetonitrile for 3 min without purification step. The chromatographic separation of the six m…
Effect of high hydrostatic pressure (HPP) and pulsed electric field (PEF) technologies on reduction of aflatoxins in fruit juices
Abstract The high demand of fresh-like products to meet the fruits and vegetables serving encouraged the implementation of non-thermal food processing techniques, such as high pressure processing (HPP) and pulsed electric fields (PEF), with low impact on nutritional components. The aim of the present work is to evaluate the application of HPP and PEF techniques as useful decontamination tool for aflatoxins (AFs) reduction in grape juice. Spiked grape juice samples with AFs treated by PEF or HPP were extracted using dispersive liquid-liquid microextraction (DLLME) and determined by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS-IT). Reduction percentages of 14–29% have b…
Mind the gap in the knowledge of the potential food applications of ultrasound based on its mechanism of action
Abstract Ultrasound is recognized as one of the alternative green technologies that are used in food technology over the last decades. It is used for several purposes, such as analysis, preservation, emulsification, crystallization, homogenization, extraction, thawing, filtration, and drying. To achieve these purposes, ultrasound mainly consists of the application of acoustic waves generating mechanical and chemical phenomena that are fundamentally different compared with those applied in conventional methods. The principle of this technology aims to save energy, decreases the processing time, and improves the quality, safety, and shelf life of food products. In this regard, this book chapt…
Multiresidue analysis of pesticides in honey by quechers and gas chromatography mass spectrometry in tandem
Evolution of emerging Fusarium mycotoxins contents throughout the shelf-life period of food
which is cooked by steaming. It has been historically eaten in North African countries but nowadays its consumption is widely extended all around the world. As a cereal-based food, semolina is highly susceptible to contamination by mycotoxin-producing fungi. The presented procedure involves a modified QuEChERSbased extraction of 24 mycotoxins (15-ADON, 3-ADON, AFLAB1, AFLAB2, AFLAG1, AFLAG2, BEA, DON, DAS, ENA, ENA1, ENB, ENB1, FB1, FB2, FB3, FUSX, HT-2, NEO, NIV, OTA, STG, T2, ZEA) produced by Aspergillus, Penicillum and Fusarium fungi. The validation was performed by analyzing recovery samples at three different spiked concentrations with four replicates (n=4) at each concentration. Recov…
Reactive oxygen species induced by beauvericin, patulin and zearalenone in CHO-K1 cells
The cytotoxic effects of mycotoxins, induction of reactive oxygen species (ROS) and generation of lipid peroxidation products in CHO-K1 cells were determined as function of increasing time of exposure and concentrations of beauvericin (BEA), patulin (PAT) and zearalenone (ZEA). The end points were evaluated after 24h of exposure, by the tetrazolium salt (MTT) and neutral red (NR) assays. The IC(50) values obtained on the MTT and NR assays ranged from 0.69 to 79.40 microM and 4.40 to 108.76 microM, respectively. To determine the intracellular production of ROS, the intensity of fluorescence emitted from the probe H(2)-DCFDA was measured. The relative intensity of fluorescence from cells incu…
Risk assessment of beauvericin, enniatins and fusaproliferin present in follow-up infant formula by in vitro evaluation of the duodenal and colonic bioaccessibility
Abstract In this study, 72 samples of follow-up infant formula of Spanish origin were analyzed for the presence of the mycotoxins beauvericin (BEA), enniatins (ENs) (A, A1, B, B1), and fusaproliferin (FUS). The samples analyzed were extracted three times with ethyl acetate and then the mycotoxins were identified and quantified using a liquid chromatography (LC) coupled to a diode array detector (DAD). The positive samples analyzed in this study were digested through a simulated gastrointestinal digestion model, which permit to simulate the physiological condition of the human gastrointestinal tract (duodenal and colonic compartments) in order to assess the bioaccessibility of the bioactive …
Simultaneous determination of mycotoxin in commercial coffee
Abstract Mycotoxins are secondary metabolites produced by filamentous fungi that usually contaminate food products. Coffee is a natural product susceptible to mycotoxin contamination. The present study evaluates the presence of nivalenol, deoxynivalenol, T-2 and HT-2 Toxin, diacetoxyscirpenol, aflatoxin B 1 , aflatoxin B 2 , aflatoxin G 1 , aflatoxin G 2 , fumonisin B 1 , fumonisin B 2 , ochratoxin A, zearalenone, enniatin A, enniatin A 1 , enniatin B, enniatin B 1 , and beauvericin in coffee samples, using liquid chromatography tandem mass spectrometry (LC-MS/MS). The results show that zearalenone was not present in any sample. In the positive samples the contents of fumonisins ranged from…
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…
High-performance liquid chromatographic determination of Maillard compounds in store-brand and name-brand ultra-high-temperature-treated cows' milk.
Furosine and furfural products of the Maillard reaction are used as specific indicators of the effect of heating treatments on milk quality. Their contents were measured in representative samples of store- and name-brand ultra-high-temperature-treated milks using RP-HPLC with UV detection. Furosine contents ranged from 40.32 to 50.67 and from 65.48 to 310.58 mg/100 g protein in name- and store-brand milks, respectively. Of the furfurals, only hydroxymethylfurfural was detected. The free hydroxymethylfurfural contents of store-brand milks ranged from 0.22 to 1.70 mg/100 g protein. Total hydroxymethylfurfural contents ranged from 0.29 to 0.41 and from 0.72 to 2.21 mg/100 g protein, for name- …
Ultrasound Processing: A Sustainable Alternative
Abstract The UN’s 2030 program for sustainable development, and the society growing demand of greener alternatives, encourage global food industry to develop affordable, safe, effective, innovative, and ecologically processing technologies. Among them, ultrasound technique links with green chemistry and eco-friendly characteristics. This technology does not involve chemical solvents, being a sustainable alternative to industry. Moreover, it minimally affects sensorial and health promoting attributes of food products. Comparing with conventional processes, ultrasound provides some benefits to achieve sustainability goals, it reduces the processing time and cost, simplifies the manipulation, …
High-performance liquid chromatographic determination of furfural compounds in infant formulas
Furfural contents in adapted and follow-up infant formulas were measured by RP-HPLC. The evolution of furfural compound contents during storage (a year at 20 and 37 °C) was studied. 2-Furylmethylketone and 5-methyl-2-furaldehyde were not detectable in analysed samples. The differences in the furfural compounds at point zero between both infant formulas has to be ascribed to the differences in protein and iron contents. An increase in free 5-hydroxymethyl-2-furfuraldehyde (HMF), 2-furaldehyde (F) and HMF+F contents was observed in all samples, although the differences were not statistically significant. The storage temperature affected the total HMF content and the storage time affected the …
Mycotoxins and their consequences in aquaculture: A review
Fish consumption has been increasing worldwide, mainly due to the availability, access and price in relation to other kinds of meat consumption, such as beef, pork, and poultry. Consequently, some concerns begin to emerge, primarily regarding the quality of fish available in the market. Residues could be present in any product of animal origin causing economic losses and putting into a risk human and animal health. Food contamination by mycotoxins is a risk to human and animal health, and it is responsible for significant economic losses. It's very difficult to prove that a disease is a mycotoxicosis, and even when mycotoxins are detected, it is not easy to show that they are the etiologica…
Multi‐Mycotoxin Analysis in Durum Wheat Pasta by Liquid Chromatography Coupled to Quadrupole Orbitrap Mass Spectrometry
A simple and rapid multi‐mycotoxin method for the determination of 17 mycotoxins simultaneously is described in the present survey on durum and soft wheat pasta samples. Mycotoxins included in the study were those mainly reported in cereal samples: ochratoxin‐A (OTA), aflatoxin B1 (AFB1), zearalenone (ZON), deoxynivalenol (DON), 3‐and 15‐acetyl‐deoxynivalenol (3‐AcDON and 15‐AcDON), nivalenol (NIV), neosolaniol (NEO), fusarenon‐X, (FUS‐X), T‐2 toxin (T‐2) and HT‐2 toxin (HT‐2), fumonisin B1 and B2 (FB1 and FB2), and four emerging mycotoxins: three enniatins (ENA, ENA1, and ENB), and beauvericin (BEA). Twenty‐nine samples were analyzed to provide an overview on mycotoxin presence: 27 samples…
Quantitative determination of octylphenol, nonylphenol, alkylphenol ethoxylates and alcohol ethoxylates by pressurized liquid extraction and liquid chromatography-mass spectrometry in soils treated with sewage sludges.
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Aquaculture and its by-products as a source of nutrients and bioactive compounds
Underutilized marine resources (e.g., algae, fish, and shellfish processing by-products), as sustainable alternatives to livestock protein and interesting sources of bioactive compounds, have attracted the attention of the researchers. Aquatic products processing industries are growing globally and producing huge amounts of by-products that often discarded as waste. However, recent studies pointed out that marine waste contains several valuable components including high-quality proteins, lipids, minerals, vitamins, enzymes, and bioactive compounds that can be used against cancer and some cardiovascular disorders. Besides, previously conducted studies on algae have shown the presence of some…
Multimycotoxin LC-MS/MS Analysis in Tea Beverages after Dispersive Liquid-Liquid Microextraction (DLLME).
The aim of the present study was to develop a multimycotoxin liquid chromatography tandem mass spectrometry (LC-MS/MS) method with a dispersive liquid-liquid microextraction procedure (DLLME) for the analysis of AFs, 3aDON, 15aDON, NIV, HT-2, T-2, ZEA, OTA, ENNs, and BEA in tea beverages and to evaluate their mycotoxin contents. The proposed method was characterized in terms of linearity, limits of detection (LODs), limits of quantification (LOQs), recoveries, repeatability (intraday precision), reproducibility (interday precision), and matrix effects to check suitability. The results show LODs in the range of 0.05-10 μg/L, LOQs in the range of 0.2-33 μg/L, and recoveries in the range of 65…
Mycotoxin Dietary Exposure Assessment through Fruit Juices Consumption in Children and Adult Population
Consumption of fruit juice is becoming trendy for consumers seeking freshness and high vitamin and low caloric intake. Mycotoxigenic moulds may infect fruits during crop growth, harvest, and storage leading to mycotoxin production. Many mycotoxins are resistant to food processing, which make their presence in the final juice product very likely expected. In this way, the presence of 30 mycotoxins including aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1), aflatoxin G2 (AFG2), alternariol (AOH), alternariol monomethyl ether (AME), Ochratoxin A (OTA), fumonisin B1 (FB1), fumonisin B2 (FB2), enniatin A (ENNA), enniatin A1 (ENNA1), enniatin B (ENNB), enniatin B1 (ENNB1), beauverici…
Natural occurrence of emerging Fusarium mycotoxins in feed and fish from aquaculture.
A new analytical method for the simultaneous determination of enniatins (ENs) and beauvericin (BEA) in fish feed and fish tissues by liquid chromatography coupled to mass spectrometry with linear ion trap (LC-MS/MS-LIT) was developed. Results showed that the developed method is precise and sensitive. The presence of emerging Fusarium mycotoxins, ENs and BEA, was determined in samples of aquaculture fish and feed for farmed fish, showing that all feed samples analyzed were contaminated with mycotoxins, with 100% coexistence. In aquacultured fish samples, the highest incidence was found in edible muscle and liver. As for the exposure assessment calculated, it was found that average consumer i…
Mycotoxin Incidence in Some Fish Products: QuEChERS Methodology and Liquid Chromatography Linear Ion Trap Tandem Mass Spectrometry Approach
The inclusion of vegetal raw materials in feed for fish farming has increased the risk of mycotoxin occurrence in feed, as well as in edible tissues from fish fed with contaminated feed, due to the carry-over to muscle portions. Therefore, the objective of this study was to evaluate the occurrence of 15 mycotoxins in processed fish products, which are commonly consumed, such as smoked salmon and trout, different types of sushi, and gula substitutes. A QuEChERS method was employed to perform the mycotoxin extraction from fish samples. For mycotoxin identification and quantitation, the selected technique was the liquid chromatography-tandem mass spectrometry linear ion trap (LC-MS/MS-LIT). Sm…
Whole blood selenium content in pregnant women
The selenium content in the blood of pregnant women in the Valencian Community, Spain was determined until the end of gestation in order to assess its evolution and detect possible differences in relation to the values corresponding to non-pregnant women of fertile age. A total of 158 blood samples were obtained from 137 pregnant women. Samples were classified as: (a) first; (b) second; and (c) third trimester. Selenium was determined by a flow injection hydride atomic absorption spectrometric method (Seronorm whole blood was used as a quality control check). The selenium values obtained for the three trimesters followed a Gaussian distribution. The intervals for mean found were: (a) 75.7-8…
Occurrence of Mycotoxins in Botanical Dietary Supplement Infusion Beverages.
The aim of the present work was to study the occurrence of mycotoxins [aflatoxins (1-4), 3-acetyldeoxyniavlenol (5), 15-acetyldeoxynivalenol (6), nivalenol (7), HT-2 (8), T-2 (9), ochratoxin A (10), zearalenone (11), enniatin A (12), enniatin A1 (13), enniatin B (14), enniatin B1 (15), and beauvericin (16)] present in potable products derived from herbal teas. Analysis was carried out by liquid chromatography coupled to ion-trap tandem mass spectrometry (LC-MS/MS-IT) after a dispersive liquid-liquid microextraction procedure (DLLME) was conducted. The DLLME method was applied to 52 commercial samples of chamomile, chamomile with anise, chamomile with honey, linden, pennyroyal mint, thyme, v…
Multimycotoxin analysis in water and fish plasma by liquid chromatography-tandem mass spectrometry
High performance liquid chromatography-mass spectrometry was used for the determination of 15 mycotoxins in water and fish plasma samples, including aflatoxins, fumonisins, ochratoxin A, sterigmatocistin, fusarenon-X and emerging Fusarium mycotoxins. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a sample treatment for the simultaneous extraction of mycotoxins. Results showed differences in recovery assays when different extraction solvents were employed. Ethyl acetate showed better recoveries for the major part of mycotoxins analyzed, except for aflatoxins B2, G1 and G2, which showed better recoveries when employing chloroform as extractant solvent. Fumonisi…
High Pressure Processing Impact on Alternariol and Aflatoxins of Grape Juice and Fruit Juice-Milk Based Beverages.
High-pressure processing (HPP) has emerged over the last 2 decades as a good alternative to traditional thermal treatment for food safety and shelf-life extension, supplying foods with similar characteristics to those of fresh products. Currently, HPP has also been proposed as a useful tool to reduce food contaminants, such as pesticides and mycotoxins. The aim of the present study is to explore the effect of HPP technology at 600 MPa during 5 min at room temperature on alternariol (AOH) and aflatoxin B1 (AFB1) mycotoxins reduction in different juice models. The effect of HPP has also been compared with a thermal treatment performed at 90 °C during 21 s. For this, different juice models, or…
Emerging Fusarium mycotoxins in organic and conventional pasta collected in Spain
Abstract One of the main sources of emerging Fusarium mycotoxins in human nutrition is the cereals and cereal products. In this study, an analytical method to determine enniatins A, A1, B and B1 (ENs), beauvericin (BEA) and fusaproliferin (FUS) based on Ultra-Turrax extraction followed by liquid chromatography coupled to triple quadrupole mass spectrometer detector (MS/MS QqQ), was applied for the analysis of pasta. For this purpose, 114 commercial samples of pasta were acquired from supermarkets located in Valencia. The results showed higher frequencies of contamination in organic pasta than in conventional pasta, while the concentration levels were variable for both types of pasta. In pos…
Fluorometric determination of chemically available lysine: adaptation, validation and application to different milk products.
A spectrophotometric method based on the reaction between available lysine and ortho-phthaldialdehyde (OPA) was adapted and validated for fluorometric determination of the chemically available lysine contents in milk matrices (UHT and conventional in-bottle sterilized cow milk, milk-based infant formulas and infant formula ingredients). The values of the analytical parameters show its usefulness as a routine method (linearity, r = 0.9992; detection limit, 0.0066 mg/mL assay; accuracy, 99-108%; precision, intra-day 2.1-5.9% and inter-day 3.5 10.2%). No statistically significant differences (p < 0.05) were found between the values obtained with the adapted method and those obtained applying t…
The potential of pulsed electric fields to reduce pesticides and toxins
Abstract Several studies have demonstrated the feasibility of pulsed electric fields (PEF) for different applications in the food industry. PEF technology is a valuable tool to improve functionality, extractability, and recovery of nutritionally valuable compounds as well as bioavailability of micronutrients and components in a diverse variety of foods. Moreover, some studies have shown the potential of PEF treatments to reduce the formation of food processing contaminants, pesticides, and toxins. This opens the doors to new PEF applications in the food industry. Recently, scientists explored the possibility of removing harmful chemical, such as pesticides and toxins, from food commodity by…
Influence of the making and cooking pasta on enniatins contents
Development of a new method for the simultaneous determination of 21 mycotoxins in coffee beverages by liquid chromatography tandem mass spectrometry
Abstract A new method for the simultaneous detection of 21 mycotoxins (ochratoxin A, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, sterigmatocystin, nivalenol, deoxynivalenol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, diacetoxyscirpenol, neosolaniol, HT-2 toxin, T-2 toxin, fumonisin B1, fumonisin B2, enniatin A, enniatin A1, enniatin B, enniatin B1, and beauvericin) in coffee beverages was internally validated. The method is based on liquid/liquid extraction with a mixture of ethyl acetate/formic acid (95:5 v/v) and detection using triple quadrupole (QqQ) and ion trap (IT) liquid chromatography tandem mass spectrometry. The limits of detection and quantification were 0.02…
Presence of mycotoxins in ready-to-eat food and subsequent risk assessment
Abstract A study on a set of ready-to-eat meals (n = 328) based on cereals, legumes, vegetables, fish and meat was carried out to determine the natural presence of twenty-seven mycotoxins by both liquid chromatography and gas chromatography coupled mass spectrometry in tandem (MS/MS) after QuEChERS extraction. The occurrence of mycotoxins was headed by cereal samples with 35% of samples contaminated by at least one mycotoxin followed by vegetables (32%), legumes (15%) and lastly, 9% of fish and meat samples were contaminated. DON was the most detected mycotoxin in vegetables, meat, fish and cereals with an incidence of 13% 18% 19% and 60%, respectively, and the highest mean levels were foun…
Protective effect against mycotoxin occurrence of different additives in smoked fish
Fermentation in fish and by-products processing: an overview of current research and future prospects
Fish industry has been growing continuously over the last decades and generates huge amounts of by-products. These by-products come from fish head, skin, bones, thorns, and viscera. Part of them are processed for feed, collagen and oil production, and to a lesser extent to produce biofuels and fertilizers, but many other high-value bioactive compounds can be recovered. Fish fermentation, which is traditionally used to increase fish shelf-life, results into the formation of bacteria metabolites of interest. Applied to by-products, fermentation increases the quality of protein hydrolysates, oil and produces antioxidant compounds. This technology, which is safe, environmental-friendly and poor…
Simultaneous determination of bisphenol A, octylphenol, and nonylphenol by pressurised liquid extraction and liquid chromatography–tandem mass spectrometry in powdered milk and infant formulas
Abstract A new analytical method, using pressurised liquid extraction (PLE) and liquid chromatography–tandem mass spectrometry (LC–MS/MS), was developed for the simultaneous determination of bisphenol A (BPA), octylphenol (OP) and nonylphenol (NP) in powdered infant formulas (IF) and powdered skimmed milk (PM). The analytes were extracted by PLE, using this optimised conditions: ethyl acetate as solvent, 70 °C of temperature, reversed-phase silica C18 as dispersing agent and three cycles of extraction. The extracts were then injected in LC–MS/MS using a Gemini C18 column and a mixture of 5% water and 95% methanol/acetonitrile, both with 0.1% ammonia, as a mobile phase. Recoveries at differe…
Dietary exposure assessment to mycotoxins through total diet studies. A review
Mycotoxins are secondary metabolites of fungi that contaminate food in several stages and their increasing presence in food chain demand further control. Assessment of mycotoxins human exposure through processed diet is an important component of food safety strategies. The present review explores and summarises total diet studies (TDS) carried out in different countries focusing on mycotoxins determination. TDS were classified by samples preparation, mycotoxins analysis and dietary exposure evaluation. Most of reviewed TDS performed multi-mycotoxins analysis in composite samples mainly, prepared taking into account local culinary habits. High performance liquid chromatography coupled with f…
Extraction of Antioxidant Compounds and Pigments from Spirulina (Arthrospira platensis) Assisted by Pulsed Electric Fields and the Binary Mixture of Organic Solvents and Water
The application of pulsed electric fields (PEF) is an innovative extraction technology promoting cell membrane electroporation, thus allowing for an efficient recovery, from an energy point of view, of antioxidant compounds (chlorophylls, carotenoids, total phenolic compounds, etc.) from microalgae. Due to its selectivity and high extraction yield, the effects of PEF pre-treatment (3 kV/cm, 100 kJ/kg) combined with supplementary extraction at different times (5–180 min) and with different solvents (ethanol (EtOH)/H2O, 50:50, v/v
Revision: Indicadores del deterioro de la calidad proteica y del valor nutritivo de la leche / Review: Indicators of damage of protein quality and nutritional value of milk
The nutritional value of milk can be negatively affected by thermal treatments. The quality of the proteins can be modified as a consequence of a set of reactions, the most important of which are the interactions between protein and carbohydrates, also known as Maillard reactions. These reactions can also occur when the storage conditions of moisture and temperature are unfavorable. The differ ent thermal treatments involved in processing milk (pasteurization, sterilization, drying, etc.) lead to different steps of the Maillard reaction and therefore to the formation of different compounds that can be useful as chemical markers of milk alteration, or more exactly of protein alteration. Est…
Enniatin B metabolites in liver and tissues of gilthead sea bream (Sparus aurata)
Dietary Exposure to Mycotoxins through Alcoholic and Non-Alcoholic Beverages in Valencia, Spain
The present study investigated the presence of 30 mycotoxins in 110 beverage samples of beer, wine, cava, and cider purchased in Valencia (Spain). A validated method based on dispersive liquid–liquid microextraction and chromatographic methods coupled with tandem mass spectrometry was applied. The method showed satisfactory recoveries ranging from 61 to 116% for the different beverages studied. The detection and quantification limits ranged from 0.03 to 2.34 µg/L and 0.1 to 7.81 µg/L, respectively. The results showed that beer samples were the most contaminated, even with concentrations ranging from 0.24 to 54.76 µg/L. A significant presence of alternariol was found in wine, which reached c…
Recent advances in the application of innovative food processing technologies for mycotoxins and pesticide reduction in foods
Abstract Background Agricultural products are a vital component of the human diet. However, these products can be contaminated by health-threatening pesticides and mycotoxins due to improper farming and storage practices. Besides, pesticide pollution can be also regarded as environmental pollution and pesticide reduction is among the Sustainable Development Goals (SDGs). While these hazardous chemicals are stable during several traditional food processing, innovative food processing technologies, including high-pressure processing (HPP), pulsed electric fields (PEF), cold plasma (CP), supercritical carbon dioxide (SC-CO2), and ultrasound (USN) processing, have been found to have good potent…
Optimization of selenium determination in human milk and whole blood by flow injection hydride atomic absorption spectrometry.
abstract A flow injection hydride atomic absorption spectrometry (FI-HAAS) method was developed for determining selenium in human milk and whole blood after microwave digestion of the sample. The sample (2 mL human milk or 0.25 mL blood) was introduced into the microwave vessel with 1.5 mL HN03 and 0.25 mL H202 and 300 W (4 min) and 600 W (4 min) were applied. The digestion was completed by heating to 140 C (2-3 h). Se (VI) was reduced to Se (IV) with hydrochloric acid. The instrumental conditions for FI-HAAS (concentrations of reducing agent and carrier acid, flow rate of argon carrier gas, and sample volume injected) were optimized. The detection limit of the proposed method was 0.23 ng/m…
Assessment of Human Exposure to Deoxynivalenol, Ochratoxin A, Zearalenone and Their Metabolites Biomarker in Urine Samples Using LC-ESI-qTOF.
Human are exposed to a wide range of mycotoxins through dietary food intake, including processed food. Even most of the mycotoxin exposure assessment studies are based on analysis of foodstuffs, and evaluation of dietary intake through food consumption patterns and human biomonitoring methods are rising as a reliable alternative to approach the individual exposures, overcoming the limitations of the indirect dietary assessment. In this study, human urine samples were analyzed, seeking the presence of deoxynivalenol (DON), ochratoxin A (OTA), zearalenone (ZEA), and their metabolites. For this purpose, 40 urine samples from female and male adult residents in the city of Valencia (Spain) were …
Investigating the in vitro catabolic fate of Enniatin B in a human gastrointestinal and colonic model
Abstract Enniatin B is an emerging mycotoxin known to present biological activity because of its ionophoric characteristics. This compound has demonstrated strong in vitro cytotoxicity against different cancer cells, also at low molecular concentrations. Its natural occurrence in food commodities and feed is highly reported world-wide, but few information is available about its stability in the human gastro-intestinal tract. The present work evaluates the catabolic fate of enniatin B upon in vitro simulated digestion and colonic fermentation. LC-MS target and untargeted analysis have been performed to quantify the extent of enniatin B degradation and the formation of catabolic products. The…
Effects of thermal processing and storage on available lysine and furfural compounds contents of infant formulas.
The Maillard reaction-related effects that thermal treatments during the manufacturing process and storage (at 20 and 37 degrees C) have on powdered adapted and follow-up milk-based infant formulas were estimated by measuring the available lysine and furfural compounds contents of raw cow milk used in manufacturing, intermediate products and formulas. A fluorimetric method was used to measure the available lysine contents, and free and total furfural compounds were determined by HPLC. Statistically significant losses in available lysine (about 20%) in the infant formulas with respect to raw milk were found. The storage period did not affect the available lysine contents of adapted formulas …
Fusarium species, chemotype characterisation and trichothecene contamination of durum and soft wheat in an area of central Italy
BACKGROUND Fusarium head blight (FHB) of wheat is an important disease causing yield losses and mycotoxin contamination. The aim of the work was to detect and characterise trichothecene producing Fusarium species in durum and soft wheat cultivated in an area of central Italy in 2009 and 2010 and to determine trichothecene contamination by LC-MS/MS in the grain. RESULTS F. graminearum s. str. was the most frequent species. In 2009, the occurrence of F. avenaceum and F. poae was higher than in 2010. Among F. graminearum strains, the 15-acetyl deoxynivalenol (15-ADON) chemotype could be found more frequently, followed by nivalenol (NIV) and 3-ADON chemotypes, while all F. culmorum isolates bel…
Evolution of available lysine and furosine contents in milk-based infant formulas throughout the shelf-life storage period
The evolution of the Maillard reaction (MR) by measuring the available lysine and furosine (FUR) contents in adapted and follow-up powdered milk-based infant formulas over the shelf-life storage period, at 20 and 37 °C, was studied. Available lysine and FUR contents were determined by fluorimetry and high-performance liquid chromatography respectively. Statistically significant differences were found between adapted and follow-up infant formulas with respect to the available lysine and FUR contents. Available lysine contents decreased significantly throughout the storage time, and the contents at 37 °C were lower than at 20 °C. A statistically significant increase in FUR contents was observ…
The potential of HPP for minimizing pesticides and toxins in food products
Abstract High-pressure (HP) treatment has emerged as a novel, additive-free food preservation technology. It has been scientifically and commercially proven that HP can produce microbially safe and stable products with improved quality characteristics such as enhanced flavor and color. Recent studies have focused on the effects of HP on health attributes and allergenic potential of foodstuff to develop the next generation of convenience foods. The contamination of produced food in various conditions along the production chain always is the point of concern. In this context, food safety is among the main health concerns worldwide on the occurrence of food contaminants such as heavy metals, h…
Development a mitigation strategy of enniatins in pasta under home-cooking conditions
The effect of pasta cooking on the enniatins (ENs) contents was evaluated in white and whole-grain pasta. The cooking of pasta was performed for 10 min in boiling water. ENs were extracted from raw and cooked pasta by Solid-Liquid extraction with acetonitrile, and from cooking water by Dispersive Liquid–Liquid Micro-Extraction (DLLME) with a mixture of acetonitrile and carbone tetrachloride. Mycotoxin analysis was performed by Liquid Chromatography coupled to Tandem Mass Spectrometry. The effect of pasta cooking has a marked influence on the reduction of ENs levels. Reductions of 98–100% for ENA, 94–95% for ENA1, 14–49% for ENB and 53–65% for ENB1 were achieved after the process. ENs were d…
Evaluation of pulsed electric field-assisted extraction on the microstructure and recovery of nutrients and bioactive compounds from mushroom (Agaricus bisporus)
Pulsed electric field (PEF) is a sustainable innovative technology that allows for the recovery of nutrients and bioactive compounds from vegetable matrices. A. bisporus was chosen for its nutritional value and the effect of PEF pretreatment was evaluated using different conditions of electric field (2–3 kV/cm), specific energy (50–200 kJ/kg) and extraction time (0–6 h) to obtain the best conditions for nutrient and bioactive compound extraction. Spectrophotometric methods were used to evaluate the different compounds, along with an analysis of mineral content by inductively coupled plasma mass spectrometry (ICP-MS) and the surface was evaluated using scanning electron microscopy (SEM). In …
Co-occurrence and risk assessment of mycotoxins in food and diet from Mediterranean area.
The contents of 14 mycotoxins were studied in samples of different cereals and cereal products from four countries of the Mediterranean region. Two hundred and sixty-five samples from Spain, Italy, Morocco and Tunisia were analysed. Samples were extracted with matrix solid-phase dispersion (MSPD) and determined by liquid chromatography-tandem mass spectrometry with a triple quadrupole mass analyser. The percentage of total samples contaminated was 53%. The frequency of contaminated samples from Spain, Italy, Tunisia and Morocco was 33%, 52%, 96% and 50%, respectively. Nivalenol and beauvericin were the most predominant mycotoxins. This is the first international report to study the presence…
High Pressure Processing Impact on Emerging Mycotoxins (ENNA, ENNA1, ENNB, ENNB1) Mitigation in Different Juice and Juice-Milk Matrices
The aim of the present study was to investigate the potential of high-pressure processing (HPP) (600 MPa during 5 min) on emerging mycotoxins, enniatin A (ENNA), enniatin A1 (ENNA1), enniatin B (ENNB), enniatin B1 (ENNB1) reduction in different juice/milk models, and to compare it with the effect of a traditional thermal treatment (HT) (90 °C during 21 s). For this purpose, different juice models (orange juice, orange juice/milk beverage, strawberry juice, strawberry juice/milk beverage, grape juice and grape juice/milk beverage) were prepared and spiked individually with ENNA, ENNA1, ENNB and ENNB1 at a concentration of 100 µg/L. After HPP and HT treatments, ENNs were extracted from treate…
Fluorescence, Browning Index, and Color in Infant Formulas during Storage
Free and total fluorescent compounds, browning index, and color formation were measured in milk-based powdered infant formulas (IF) during 2 years of storage at 20 and 37 degrees C. The excitation spectra from 415 nm emission show three peaks (ex lambda1 = 270 nm, lambda2 = 325/315 nm, lambda3 = 350 nm) and from 347 nm excitation two emission peaks (415 and 520 nm), and no wavelength shifts were observed. Temperature and time of storage exert in general no significant effect on the development of fluorescence emission intensity and browning index. However, an important increase in pentodilysine was recorded-probably because of the iron and ascorbic acid contents of the samples-as well as in…
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…
Mycotoxin Identification and In Silico Toxicity Assessment Prediction in Atlantic Salmon
The present study aimed to identify mycotoxins in edible tissues of Atlantic salmon (Salmo salar) using liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS). After using a non-targeted screening approach and a home-made spectral library, 233 mycotoxins were analyzed. Moreover, the occurrence of mycotoxins in fish filets was evaluated, and their potential toxicity was predicted by in silico methods. According to the obtained results, forty mycotoxins were identified in analyzed salmon samples, the predominant mycotoxins being enniatins (also rugulosin and 17 ophiobolins), commonly found in cereals and their by-products. Thus, mycotoxin carry-over …
Reduction of the enniatins A, A1, B, B1 by an in vitro degradation employing different strains of probiotic bacteria: Identification of degradation products by LC–MS–LIT
Abstract The degradation of the Fusarium mycotoxins ENs by 9 bacterial strains characteristic of the gastrointestinal tract like Bb. longum , Bb. bifidum , Bb. breve , Bb. adolescentes , Lb. rhamnosus , Lb. casei–casei , S. termofilus , Lb. ruminis , Lb. casei and twenty two strains of Saccharomyces cerevisiae was studied. The fermentations were carried out in the liquid medium of De Man Rogosa Sharpe (MRS) under anaerobic conditions for Bifidobacteria Streptococcus and Lactobacillus, and in Potato Dextrose Broth (PDB) for Saccharomyces strains, during 48 h. The degradation of the bioactive compounds ENs was also studied in a food system composed by wheat flour naturally contaminated by ENs…
Risk assessment of mycotoxins in coffee beverages
Degradation study of enniatins by liquid chromatography–triple quadrupole linear ion trap mass spectrometry
Abstract Enniatins A, A1, B and B1 (ENs) are mycotoxins produced by Fusarium spp. and are normal contaminants of cereals and derivate products. In this study, the stability of ENs was evaluated during food processing by simulation of pasta cooking. Thermal treatments at different incubation times (5, 10 and 15 min) and different pH (4, 7 and 10) were applied in an aqueous system and pasta resembling system (PRS). The concentrations of the targeted mycotoxins were determined using liquid chromatography coupled to tandem mass spectrometry. High percentages of ENs reduction (81–100%) were evidenced in the PRS after the treatments at 5, 10 and 15 min of incubation. In contrast to the PRS, an im…
Effects of technological processes on enniatin levels in pasta
BACKGROUND Potential human health risks posed by enniatins (ENs) require their control primarily from cereal products, creating a demand for harvesting, food processing and storage techniques capable to prevent, reduce and/or eliminate the contamination. In this study, different methodologies to pasta processing simulating traditional and industrial processes were developed in order to know the fate of the mycotoxin ENs. The levels of ENs were studied at different steps of pasta processing. The effect of the temperature during processing was evaluated in two types of pasta (white and whole-grain pasta). Mycotoxin analysis was performed by LC-MS/MS. RESULTS High reductions (up to 50% and 80%…
Antibacterial activity of the emerging Fusarium mycotoxins enniatins A, A1, A2, B, B1, and B4 on probiotic microorganisms
Abstract Enniatins (ENs) are secondary metabolites produced by several Fusarium strains, chemically characterized as N-methylated cyclohexadepsipeptides. These compounds are known to act as antifungal and antibacterial agents, but they also possess anti-insect and phytotoxic properties. In this study, the antimicrobial effect of pure fractions of the bioactive compounds ENs A, A 1 , A 2 , B, B 1 , and B 4 was tested towards nine probiotic microrganisms, twenty-two Saccharomyces cerevisiae strains and nine Bacillus subtilis strains. Antimicrobial analyses were carried out the disc-diffusion method using ENs concentrations ranging from 0.2 to 20,000 ng. Plates were incubated for 24 h at 37 °C…
Evaluation of Mycotoxin Residues on Ready-to-Eat Food by Chromatographic Methods Coupled to Mass Spectrometry in Tandem
Simultaneous determination of twenty-seven mycotoxins in ready-to-eat food samples using &ldquo
Effect of different thermal processes in the reduction of enniatins in fish tissues
Analysis of mycotoxins in coffee and risk assessment in Spanish adolescents and adults.
Mycotoxins are toxic compounds produced by fungal secondary metabolism that cause toxicological effects. Coffee is a highly popular beverage that is susceptible to contamination by mycotoxigenic fungi. The aim of the present study was to determine the presence of the following 21 mycotoxins in coffee using liquid chromatography tandem mass spectrometry (LC-MS/MS-IT): aflatoxin B1, B2, G1 and G2; ochratoxin A; nivalenol; deoxynivalenol; 3-acetyldeoxynivalenol; 15-acetyldeoxynivalenol; diacetoxyscirpenol; neosolaniol; T-2 and HT-2 toxin; sterigmatocystin; enniatin A, A1, B, and B1; beauvericin; and fumonisin B1 and B2. We aimed to determine differences by coffee process (coffee maker, electri…
Innovative Green Technologies of Intensification for Valorization of Seafood and Their By-Products
The activities linked to the fishing sector generate substantial quantities of by-products, which are often discarded or used as low-value ingredients in animal feed. However, these marine by-products are a prominent potential good source of bioactive compounds, with important functional properties that can be isolated or up-concentrated, giving them an added value in higher end markets, as for instance nutraceuticals and cosmetics. This valorization of fish by-products has been boosted by the increasing awareness of consumers regarding the relationship between diet and health, demanding new fish products with enhanced nutritional and functional properties. To obtain fish by-product-derived…