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Showing papers in "Food Additives and Contaminants Part A-chemistry Analysis Control Exposure & Risk Assessment in 2012"


Journal ArticleDOI
Peter M. Scott1
TL;DR: Intentional binding of fumonisins to cholestyramine has been demonstrated in vivo and is a potential means of detoxification of animal feed.
Abstract: Fumonisins are well known mycotoxins produced by Fusarium verticillioides, F. proliferatum and other Fusarium species. Many new fumonisins and fumonisin-like compounds have been detected by mass spectrometry in cultures of F. verticillioides. Recently, fumonisins B2 and B4 were produced by Aspergillus niger isolated from coffee and fumonisin B2 in A. niger from grapes. Fumonisin B2 was itself detected in coffee beans, wine and beer, adding to the list of foodstuffs and feedstuffs other than corn (maize) and sorghum in which fumonisins have been found in recent years. Fumonisin B1 (FB1) can bind to proteins (PB FB1) and to other matrix components during food processing involving heat. The occurrence of bound fumonisins in processed corn foods is common. Another type of binding (or association) relates to observed instability of fumonisins in rice flour, corn starch and corn meal at room temperature; this can affect the immunoaffinity column clean-up procedure in analysis of naturally contaminated starch-co...

153 citations


Journal ArticleDOI
TL;DR: The results showed advancements of sowing date of spring cereals by 1–3 weeks depending on climate model and region within Europe, and the responses of wheat and oats were largest for the period from flowering to maturity.
Abstract: The phenological development of cereal crops from emergence through flowering to maturity is largely controlled by temperature, but also affected by day length and potential physiological stresses. Responses may vary between species and varieties. Climate change will affect the timing of cereal crop development, but exact changes will also depend on changes in varieties as affected by plant breeding and variety choices. This study aimed to assess changes in timing of major phenological stages of cereal crops in Northern and Central Europe under climate change. Records on dates of sowing, flowering, and maturity of wheat, oats and maize were collected from field experiments conducted during the period 1985–2009. Data for spring wheat and spring oats covered latitudes from 46 to 64°N, winter wheat from 46 to 61°N, and maize from 47 to 58°N. The number of observations (site–year–variety combinations) varied with phenological phase, but exceeded 2190, 227, 2076 and 1506 for winter wheat, spring wheat, spring ...

151 citations


Journal ArticleDOI
TL;DR: The method allowed the simultaneous determination of 13 Fusarium mycotoxins in a one-step chromatographic run using a Waters Acquity UPLC system coupled to a Quattro Premier XE mass spectrometer, in good agreement with the criteria mentioned in Commission Regulation (EC) No. 401/2006.
Abstract: An LC-MS/MS method was developed and validated for the simultaneous determination of deoxynivalenol, zearalenone, T-2-toxin, HT-2-toxin and metabolites, including 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, deoxynivalenol-3-glucoside, alpha-zearalenol, beta-zearalenol, zearalenone-4-glucoside, alpha-zearalenol-4-glucoside, beta-zearalenol-4-glucoside and zearalenone-4-sulfate in maize, wheat, oats, cornflakes and bread. Extraction was performed with acetonitrile/water/acetic acid (79/20/1, v/v/v) followed by a hexane defatting step. After filtration, the extract was evaporated and the residue was redissolved in mobile phase for injection. The mobile phase, which consisted of a mixture of methanol and water with 10 mM ammonium acetate, was adjusted to pH 3 with glacial acetic acid. A sample clean-up procedure was not included because of the low recoveries of free and masked mycotoxins and their differences in polarity. The method allowed the simultaneous determination of 13 Fusarium mycotoxins in a one-step chromatographic run using a Waters Acquity UPLC system coupled to a Quattro Premier XE mass spectrometer. The method was validated for several parameters such as linearity, apparent recovery, limit of detection, limit of quantification, precision, expanded measurement uncertainty and specificity. The limits of detection varied from 5 to 13 ng g(-1); those for the limit of quantification from 10 to 26 ng g(-1). The results of the performance characteristics of the developed LC-MS/MS method were in good agreement with the criteria mentioned in Commission Regulation (EC) No. 401/2006. Thirty samples of a variety of food and feed matrices were sampled and analysed between July 2010 and January 2011.

143 citations


Journal ArticleDOI
TL;DR: This review will give an overview of the current state of the art, focusing particularly on the suitability of the most used techniques for the size measurement of nanoparticles when addressing this new definition of nanomaterials.
Abstract: Nanoparticles are already used in several consumer products including food, food packaging and cosmetics, and their detection and measurement in food represent a particularly difficult challenge. In order to fill the void in the official definition of what constitutes a nanomaterial, the European Commission published in October 2011 its recommendation on the definition of ‘nanomaterial’. This will have an impact in many different areas of legislation, such as the European Cosmetic Products Regulation, where the current definitions of nanomaterial will come under discussion regarding how they should be adapted in light of this new definition. This new definition calls for the measurement of the number-based particle size distribution in the 1–100 nm size range of all the primary particles present in the sample independently of whether they are in a free, unbound state or as part of an aggregate/agglomerate. This definition does present great technical challenges for those who must develop valid and compati...

133 citations


Journal ArticleDOI
TL;DR: Agronomic factors were related to the infestation of Fusarium species and the concentration of mycotoxins and it is reasonable to conclude that farming system (organic versus conventional) impacts FUSarium infestation, and that organic management tends to reduce Fus aquarium and mycotoxin concentrations.
Abstract: A total of 602 samples of organically and conventionally grown barley, oats and wheat was collected at grain harvest during 2002–2004 in Norway. Organic and conventional samples were comparable pairs regarding cereal species, growing site and harvest time, and were analysed for Fusarium mould and mycotoxins. Agronomic and climatic factors explained 10–30% of the variation in Fusarium species and mycotoxins. Significantly lower Fusarium infestation and concentrations of important mycotoxins were found in the organic cereals. The mycotoxins deoxynivalenol (DON) and HT-2 toxin (HT-2) constitute the main risk for human and animal health in Norwegian cereals. The impacts of various agronomic and climatic factors on DON and HT-2 as well as on their main producers F. graminearum and F. langsethiae and on total Fusarium were tested by multivariate statistics. Crop rotation with non-cereals was found to reduce all investigated characteristics significantly – mycotoxin concentrations as well as various Fusarium inf...

128 citations


Journal ArticleDOI
TL;DR: Results of a study in Shanghai men strongly support a causal relationship between HCC risk and the presence of biomarkers for aflatoxin and HBV infection, and also show that the two risk factors act synergistically.
Abstract: The aflatoxins were discovered in toxic peanut meal causing "turkey X" disease, which killed large numbers of turkey poults, ducklings and chicks in the UK in the early 1960s. Extracts of toxic feed induced the symptoms in experimental animals, and purified metabolites with properties identical to aflatoxins B(1) and G(1) (AFB(1) and AFG(1)) were isolated from Aspergillus flavus cultures. Structure elucidation of aflatoxin B(1) was accomplished and confirmed by total synthesis in 1963. AFB(1) is a potent liver carcinogen in rodents, non-human primates, fish and birds, operating through a genotoxic mechanism involving metabolic activation to an epoxide, formation of DNA adducts and, in humans, modification of the p53 gene. Aflatoxins are unique among environmental carcinogens, in that elucidation of their mechanisms of action combined with molecular epidemiology provides a foundation for quantitative risk assessment; extensive evidence confirms that contamination of the food supply by AFB(1) puts an exposed population at increased risk of developing hepatocellular carcinoma (HCC). Molecular biomarkers to quantify aflatoxin exposure in individuals were essential to link aflatoxin exposure with liver cancer risk. Biomarkers were validated in populations with high HCC incidence in China and The Gambia, West Africa; urinary AFB(1)-N (7)-Guanine excretion was linearly related to aflatoxin intake, and levels of aflatoxin-serum albumin adducts also reflected aflatoxin intake. Two major cohort studies employing aflatoxin biomarkers identified their causative role in HCC etiology. Results of a study in Shanghai men strongly support a causal relationship between HCC risk and the presence of biomarkers for aflatoxin and HBV infection, and also show that the two risk factors act synergistically. Subsequent cohort studies in Taiwan confirm these results. IARC classified aflatoxin as a Group 1 human carcinogen in 1993, based on sufficient evidence in humans and experimental animals indicating the carcinogenicity of naturally occurring mixtures of aflatoxins, aflatoxin B(1), G(1) and M(1). Aflatoxin biomarkers have also been used to show that primary prevention to reduce aflatoxin exposure can be achieved by low-technology approaches at the subsistence farm level in sub-Saharan Africa. Also, in residents of Qidong, China, oral dosing with chlorophyllin, a chlorophyll derivative, prior to each meal led to significant reduction in aflatoxin-DNA biomarker excretion, supporting the feasibility of preventive measures to reduce HCC risk in populations experiencing unavoidable aflatoxin exposure. The systematic, comprehensive approach used to create the total aflatoxin database justifies optimism for potential success of preventive interventions to ameliorate cancer risk attributable to aflatoxin exposure. This strategy could serve as a template for the development, validation and application of molecular and biochemical markers for other carcinogens and cancers as well as other chronic diseases resulting from environmental exposures.

120 citations


Journal ArticleDOI
TL;DR: A series of model reactions mimicking palm oil deodorisation has been conducted with pure acylglycerols in the presence or absence of either organic or inorganic chlorine-containing compounds, showing that the bulk of MCPD diesters are formed above 200°C through the reaction of organochlorines with triacyl glycerols (TAG).
Abstract: Monochloropropanediol (MCPD) fatty acid esters are process contaminants generated during the deodorisation of edible oils. In particular, MCPD diesters are found in higher abundance in refined palm oil than other edible oils. In the present study, a series of model reactions mimicking palm oil deodorisation has been conducted with pure acylglycerols in the presence or absence of either organic or inorganic chlorine-containing compounds. Results showed that the bulk of MCPD diesters are formed above 200°C through the reaction of organochlorines with triacylglycerols (TAG). Additional experiments confirmed that this reaction can be initiated during palm oil deodorisation by hydrogen chloride (HCl) gas evolved through the thermal degradation of organochlorines present in the oil. Therein, the majority of the ultimately produced MCPD diesters are the result of HCl reacting with TAG, via protonation, followed by the elimination of a fatty acid residue. Two possible MCPD diester formation mechanisms are highlig...

117 citations


Journal ArticleDOI
TL;DR: The results found show the necessity of monitoring rice production and the highest levels of contamination were found in rice sub-products or derived products from the husk and rice bran.
Abstract: A total of 230 samples of processed rice and its sub-products or derived products were analysed to establish the co-occurrence of several mycotoxins. Samples were analysed in the period 2007–2009 due to the outbreak of beriberi associated with the consumption of rice stored in inappropriate conditions in Brazil. According to data from the Ministry of Health, 323 cases of disease were registered in 2006, of which at least 47 cases resulted in death. The occurrence of total aflatoxin (AFT) (aflatoxin B1 + B2 + G1 + G2), ochratoxin A (OTA), zearalenone (ZON), deoxynivalenol (DON), and citreoviridin (CTV) was 58.7%, 40.0%, 45.2%, 8.3% and 22.5%, respectively. From 166 rice samples analysed, 55% had levels <0.11 µg kg−1 for AFT. For OTA and ZON, of 165 rice samples analysed, 28% and 29% were contaminated with levels from 0.20 to 0.24 µg kg−1 and from 3.6 to 290.0 µg kg−1, respectively. One sample (0.6%) was contaminated with 4872.0 µg kg−1 of ZON. A total of 91% of rice samples (n = 165) did not contain detect...

115 citations


Journal ArticleDOI
TL;DR: The predicted changes in climate towards 2050 are expected to slightly change Fusarium species composition in Northern Europe, with an increase in F. graminearum and possibly the invasion of northern parts of Central Europe and Denmark by fumonisin producers is expected.
Abstract: In Northern Europe, changes in climate may result in better growing conditions for many crops. However, the expected warmer and more humid conditions are favourable for Fusarium head blight infections on cereals. The Fusarium species prevalent in Nordic areas to date are the same as in Central Europe: F. avenaceum, F. culmorum, F. graminearum and F. poae. The prevalence of F. graminearum in cereal grain has already increased in Central Europe and is likely to increase in the North due to the expected changes in weather conditions, reduced tillage and the predicted increase in maize cultivation in Nordic countries. The possible weather extremes predispose cereals to Fusarium infections by increasing the populations of insect pests injuring plants. Adverse conditions may even create conditions suitable for F. subglutinans or F. verticilloides to infect maize and possibly other cereals in rotation in southern parts of Scandinavia. The importance of the species that infect in relatively dry conditions, F. lan...

111 citations


Journal ArticleDOI
TL;DR: The mean dietary intake of IP-TFA has decreased significantly from that cited in the 2003 US Food and Drug Administration (FDA) final rule that established labelling requirements for trans fat (4.6 g/p/d for adults).
Abstract: The dietary intake of industrially-produced trans fatty acids (IP-TFA) was estimated for the US population (aged 2 years or more), children (aged 2-5 years) and teenage boys (aged 13-18 years) using the 2003-2006 National Health and Nutrition Examination Survey (NHANES) food consumption database, market share information and trans fat levels based on label survey data and analytical data for packaged and in-store purchased foods. For fast foods, a Monte Carlo model was used to estimate IP-TFA intake. Further, the intake of trans fat was also estimated using trans fat levels reported in the US Department of Agriculture (USDA) National Nutrient Database for Standard Reference, Release 22 (SR 22, 2009) and the 2003-2006 NHANES food consumption database. The cumulative intake of IP-TFA was estimated to be 1.3 g per person per day (g/p/d) at the mean for the US population. Based on this estimate, the mean dietary intake of IP-TFA has decreased significantly from that cited in the 2003 US Food and Drug Administration (FDA) final rule that established labelling requirements for trans fat (4.6 g/p/d for adults). Although the overall intake of IP-TFA has decreased as a result of the implementation of labelling requirements, individuals with certain dietary habits may still consume high levels of IP-TFA if certain brands or types of food products are frequently chosen.

103 citations


Journal ArticleDOI
TL;DR: The presence of HT-2 toxin in oats showed a slight decreasing trends over time, but significant trends for other toxins showed an increasing presence during the last two decades, which implies that climatic conditions that are conducive for one toxin may have a decreasing effect on the other.
Abstract: This study aimed to investigate mycotoxin contamination of cereal grain commodities for feed and food production in North Western Europe during the last two decades, including trends over time and co-occurrence between toxins, and to assess possible effects of climate on the presence of mycotoxins. For these aims, analytical results related to mycotoxin contamination of cereal grain commodities, collected in the course of national monitoring programmes in Finland, Sweden, Norway and the Netherlands during a 20-year period, were gathered. Historical observational weather data, including daily relative humidity, rainfall and temperature, were obtained from each of these four countries. In total 6382 records, referring to individual sample results for mycotoxin concentrations (one or more toxins) in cereal grains were available. Most records referred to wheat, barley, maize and oats. The most frequently analysed mycotoxins were deoxynivalenol, 3-acetyl-deoxynivalenol, nivalenol, T-2 toxin, HT-2 toxin and zearalenone. Deoxynivalenol had the highest overall incidence of 46%, and was mainly found in wheat, maize and oats. Mycotoxins that showed co-occurrence were: deoxynivalenol and 3-acetyl-deoxynivalenol in oats; deoxynivalenol and zearalenone in maize and wheat; and T-2 toxin and HT-2 toxin in oats. The presence of both deoxynivalenol and zearalenone in wheat increased with higher temperatures, relative humidity and rainfall during cultivation, but the presence of nivalenol was negatively associated with most of these climatic factors. The same holds for both nivalenol and deoxynivalenol in oats. This implies that climatic conditions that are conducive for one toxin may have a decreasing effect on the other. The presence of HT-2 toxin in oats showed a slight decreasing trends over time, but significant trends for other toxins showed an increasing presence during the last two decades. It is therefore useful to continue monitoring of mycotoxins. Obtained results can be used for development of predictive models for presence of mycotoxins in cereal grains.

Journal ArticleDOI
TL;DR: DART-TOFMS is a promising tool for rapid screening of samples and establishing comprehensive (multi-sample) long-term databases may further help to improve the quality of statistical classification models.
Abstract: The rapidly growing demand for organic food requires the availability of analytical tools enabling their authentication. Recently, metabolomic fingerprinting/profiling has been demonstrated as a challenging option for a comprehensive characterisation of small molecules occurring in plants, since their pattern may reflect the impact of various external factors. In a two-year pilot study, concerned with the classification of organic versus conventional crops, ambient mass spectrometry consisting of a direct analysis in real time (DART) ion source and a time-of-flight mass spectrometer (TOFMS) was employed. This novel methodology was tested on 40 tomato and 24 pepper samples grown under specified conditions. To calculate statistical models, the obtained data (mass spectra) were processed by the principal component analysis (PCA) followed by linear discriminant analysis (LDA). The results from the positive ionisation mode enabled better differentiation between organic and conventional samples than the results from the negative mode. In this case, the recognition ability obtained by LDA was 97.5% for tomato and 100% for pepper samples and the prediction abilities were above 80% for both sample sets. The results suggest that the year of production had stronger influence on the metabolomic fingerprints compared with the type of farming (organic versus conventional). In any case, DART-TOFMS is a promising tool for rapid screening of samples. Establishing comprehensive (multi-sample) long-term databases may further help to improve the quality of statistical classification models.

Journal ArticleDOI
TL;DR: The present modelling approach represents a simplification of factors determining the distribution of cereal crops, and also some uncertainties in the data basis were apparent, and a promising way of future model improvement could be through a systematic analysis and inclusion of other variables, such as key soil properties and socio-economic conditions, influencing the comparative advantages of specific crops.
Abstract: Climate change is anticipated to affect European agriculture, including the risk of emerging or re-emerging feed and food hazards. Indirectly, climate change may influence such hazards (e.g. the occurrence of mycotoxins) due to geographic shifts in the distribution of major cereal cropping systems and the consequences this may have for crop rotations. This paper analyses the impact of climate on cropping shares of maize, oat and wheat on a 50-km square grid across Europe (45-65°N) and provides model-based estimates of the changes in cropping shares in response to changes in temperature and precipitation as projected for the time period around 2040 by two regional climate models (RCM) with a moderate and a strong climate change signal, respectively. The projected cropping shares are based on the output from the two RCMs and on algorithms derived for the relation between meteorological data and observed cropping shares of maize, oat and wheat. The observed cropping shares show a south-to-north gradient, where maize had its maximum at 45-55°N, oat had its maximum at 55-65°N, and wheat was more evenly distributed along the latitudes in Europe. Under the projected climate changes, there was a general increase in maize cropping shares, whereas for oat no areas showed distinct increases. For wheat, the projected changes indicated a tendency towards higher cropping shares in the northern parts and lower cropping shares in the southern parts of the study area. The present modelling approach represents a simplification of factors determining the distribution of cereal crops, and also some uncertainties in the data basis were apparent. A promising way of future model improvement could be through a systematic analysis and inclusion of other variables, such as key soil properties and socio-economic conditions, influencing the comparative advantages of specific crops.

Journal ArticleDOI
TL;DR: This study represents the first biomarker survey to report on the occurrence of DON biomarkers in an African population, in addition to the co-occurrence of these two potent mycotoxins.
Abstract: Mycotoxins such as the aflatoxins and deoxynivalenol (DON) are frequent contaminants of food. Aflatoxin B1 (AFB1) and DON affect the immune system and restrict growth; additionally AFB1 is carcinogenic. To date there are limited descriptive biomarker data concerning maternal exposures during pregnancy, and none on co-exposures to these mycotoxins. This survey was a cross-sectional assessment providing descriptive data on the concentrations of serum aflatoxin-albumin (AF-alb), urinary aflatoxin M1 (AFM1), and urinary DON for 98 pregnant women from Egypt, in relation to diet and socioeconomic status, during the third trimester. AF-alb was detected in 34 of 98 (35%) samples, geometric mean (GM) of positives = 4.9 pg AF-lys mg(-1) albumin (95% confidence interval (CI) = 4.1-5.8 pg mg(-1)), and AFM1 in 44 of 93 (48%) samples, GM of positives = 19.7 pg mg(-1) creatinine (95%CI = 14.8-26.3 pg mg(-1)). AF-alb and AFM1 levels were positively correlated (R = 0.276, p = 0.007). DON was detected in 63 of 93 (68%), GM of positives = 2.8 ng mg(-1) (95%CI = 2.1-3.6 ng mg(-1)). Aflatoxin and DON biomarkers were observed in 41% of the subjects concurrently. The frequency and level of these biomarkers in Egyptian women were modest compared with known high-risk countries. However, this study represents the first biomarker survey to report on the occurrence of DON biomarkers in an African population, in addition to the co-occurrence of these two potent mycotoxins. This combined exposure may be of particular concern during pregnancy given the potential of toxin transfer to the foetus.

Journal ArticleDOI
TL;DR: A procedure based on near infrared hyperspectral imaging and multivariate image analysis to detect and quantify ergot contamination in cereals was developed and it was shown that ergot can be detected using a speed of 1–100 mm/s and that a sample of 250 g can be analysed in 1 min.
Abstract: The occurrence of ergot bodies (sclerotia of Claviceps purpurea) in cereals presents a high toxicity risk for animals and humans due to the alkaloid content. To reduce this risk, the European Commission fixed an ergot concentration limit of 0.1% in all feedstuffs containing unground cereals, and a limit of 0.05% in ‘intervention’ cereals destined for humans. This study sought to develop a procedure based on near infrared hyperspectral imaging and multivariate image analysis to detect and quantify ergot contamination in cereals. Hyperspectral images were collected using an NIR hyperspectral line scan combined with a conveyor belt. All images consisted of lines of 320 pixels that were acquired at 209 wavelength channels (1100–2400 nm). To test the procedure, several wheat samples with different levels of ergot contamination were prepared. The results showed a correlation higher than 0.99 between the predicted values obtained using chemometric tools such as partial least squares discriminant analysis or supp...

Journal ArticleDOI
TL;DR: The found metal concentrations were largely below the maximum levels established at the European Union level with the exception of Cd, which exceeded the MLs in squid, red mullet, European hake and Atlantic cod.
Abstract: The presence of selected toxic heavy metals, such as cadmium (Cd), lead (Pb) and mercury (Hg), was investigated in fish and seafood products, namely, blue mussel, carpet shell clam, European squid, veined squid, deep-water rose shrimp, red mullet, European seabass, gilthead seabream, Atlantic cod, European hake, Atlantic bluefin tuna and swordfish so as to assess their human exposure through diet. Metals were detected by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS) and hydride generation atomic absorption spectrometry (Hg-AAS). Measurements of Cd, Pb and Hg were performed by means of analytical methods validated in compliance with UNI CEI EN ISO/IEC 17025 [2005. General requirements for the competence of testing and calibration laboratories. Milano (Italy): UNI Ente Nazionale Italiano di Unificazione]. The exposure assessment was undertaken matching the levels of Cd, Pb and total Hg with consumption data related to fish and seafood products selected for this purpose. In order to establish human health implications, the estimated weekly intakes (EWIs) for Cd, Pb and Hg were compared with the standard tolerable weekly intakes (TWI) for Cd and provisional tolerable weekly intakes (PTWIs) for Pb and Hg stipulated by the European Food Safety Authority (EFSA) and the Food and Agriculture Organization/World Health Organization (FAO/WHO) Joint Expert Committee on Food Additives (JECFA). The found metal concentrations were largely below the maximum levels (MLs) established at the European Union level with the exception of Cd. This metal exceeded the MLs in squid, red mullet, European hake and Atlantic cod. Squid and blue mussel showed the highest Pb concentrations which accounted for 60% and 10% of the MLs, respectively. Highest Hg levels were found in predatory fish. The concentrations of Hg in swordfish, Atlantic bluefin tuna and red mullet accounted for 50%, 30% and 30% of the MLs, respectively. The EWIs for Cd, Pb and Hg related to the consumption of fish and seafood products by the median of the Italian total population accounted for 20%, 1.5% and 10% of the standard TWI for Cd as well as PTWIs for Pb and Hg, respectively. Furthermore, the EWIs estimated using consumption data concerning Italian consumers did not exceed the standard TWI and PTWIs, except for Cd at 95th percentile.

Journal ArticleDOI
TL;DR: Three commercial mycotoxin binders containing hydrated sodium calcium aluminosilicate as the main component were used in these experiments and the possible effects of binder addition in combination with processing (pelletising) on the amount of aflatoxin B1 determined in feed were studied.
Abstract: Recently, the use of substances that can suppress or reduce absorption, promote the excretion of mycotoxins or modify their mode of action in feed, so-called mycotoxin binders, has been officially allowed in the European Union as technological feed additives. The influence of the addition of mycotoxin binders to animal feed on the analytical performance of the official methods for the determination of mycotoxins was studied and the results are presented. Where possible standardised methods for analysis were applied. Samples of 20 commercial mycotoxin binders were collected from various companies. The following mycotoxins were included in the study: aflatoxin B₁, deoxynivalenol, zearalenone, ochratoxin A, fumonisins B₁ and B₂, T-2 and HT-2 toxins. A binder (or binders combined in a group) was mixed with feed material containing the mycotoxin, and the feed material was analysed. For data evaluation, the mean values were compared by Student's t-test (an independent two-sample t-test with unequal sample sizes and equal variance). The repeatability standard deviation of each method was used as an estimate of method variability. No significant differences (p = 0.05) in mycotoxin levels between binder-free material and the material containing different binders were found. Further, the possible effects of binder addition in combination with processing (pelletising) on the amount of aflatoxin B₁ determined in feed were studied. Three commercial mycotoxin binders containing hydrated sodium calcium aluminosilicate (HSCAS) as the main component were used in these experiments. Feed samples with and without mycotoxin binders were pelletised with and without steam treatment. After pelletising, materials were analysed for AFB₁. Only the combination pelletising and a mixture of binders added at a total level of 1.2% had a significant effect (41% reduction) on the amount of AFB₁ determined.

Journal ArticleDOI
TL;DR: The results of this survey showed that the non-toxic chitin adsorbent and the allergen-free adsorbents tested could be considered as alternative fining agents to reduce OTA in red wine.
Abstract: The ability of several oenological fining agents to remove ochratoxin A (OTA) from red wine was studied. The adsorbents tested were activated sodium bentonite, egg albumin, allergen-free adsorbents (complex PVPP, plant protein and amorphous silica (complex) and high molecular weight gelatine), and the non-toxic biodegradable polymers (chitin and chitosan). Several dosages within the oenological use range were tested and the wine pH, colour parameters and polyphenol concentration impact associated with each fining agent were studied. Generally, OTA removal achieved in all treatments was higher when the adsorbent dosage increased, but the impact on wine quality also was higher. Chitin at 50 g hl(-1) removed 18% the OTA without affecting significantly the wine-quality parameters. At the highest dosage tested the gelatine and complex treatments achieved greater OTA removal (up to 39-40%) compared with bentonite, egg albumin and chitin. Moreover, the gelatine and the complex had a lower impact on colour parameters and polyphenol concentration compared with chitosan, whilst OTA was reduced to around 40%. Chitosan achieved the greatest OTA removal (67%), but it strongly affected the wine-quality parameters. Otherwise, bentonite showed a relative efficiency to remove OTA, but the CI value decreased considerably. The egg albumin treatment only removed OTA up to 16% and moreover affected strongly the CI value and CIELab parameters. The results of this survey showed that the non-toxic chitin adsorbent and the allergen-free adsorbents tested could be considered as alternative fining agents to reduce OTA in red wine.

Journal ArticleDOI
TL;DR: The Belgian population is not at risk of exceeding the established ADIs for sweeteners through an assessment of usual dietary intake of artificial sweeteners and specific consumption of table-top sweeteners.
Abstract: This study investigated whether the Belgian population older than 15 years is at risk of exceeding ADI levels for acesulfame-K, saccharin, cyclamate, aspartame and sucralose through an assessment of usual dietary intake of artificial sweeteners and specific consumption of table-top sweeteners. A conservative Tier 2 approach, for which an extensive label survey was performed, showed that mean usual intake was significantly lower than the respective ADIs for all sweeteners. Even consumers with high intakes were not exposed to excessive levels, as relative intakes at the 95th percentile (p95) were 31% for acesulfame-K, 13% for aspartame, 30% for cyclamate, 17% for saccharin, and 16% for sucralose of the respective ADIs. Assessment of intake using a Tier 3 approach was preceded by optimisation and validation of an analytical method based on liquid chromatography with mass spectrometric detection. Concentrations of sweeteners in various food matrices and table-top sweeteners were determined and mean positive concentration values were included in the Tier 3 approach, leading to relative intakes at p95 of 17% for acesulfame-K, 5% for aspartame, 25% for cyclamate, 11% for saccharin, and 7% for sucralose of the corresponding ADIs. The contribution of table-top sweeteners to the total usual intake (<1% of ADI) was negligible. A comparison of observed intake for the total population with intake for diabetics (acesulfame-K: 3.55 versus 3.75; aspartame: 6.77 versus 6.53; cyclamate: 1.97 versus 2.06; saccharine: 1.14 versus 0.97; sucralose: 3.08 versus 3.03, expressed as mg kg(-1) bodyweight day(-1) at p95) showed that the latter group was not exposed to higher levels. It was concluded that the Belgian population is not at risk of exceeding the established ADIs for sweeteners.

Journal ArticleDOI
TL;DR: The high sensitivity and specificity of the assay for CTX1B confirmed its suitability as a screening tool of CTX-like compounds in fish extracts at levels that may cause ciguatera fish poisoning.
Abstract: The ouabain/veratridine-dependent neuroblastoma (neuro-2a) cell-based assay (CBA) was applied for the determination of the presence of ciguatoxin (CTX)-like compounds in ciguatera-suspected fish samples caught in the Canary Islands. In order to avoid matrix interferences the maximal concentration of wet weight fish tissue exposed to the neuro-2a cells was set at 20 mg tissue equivalent (TE) ml−1 according to the sample preparation procedure applied. In the present study, the limit of quantification (LOQ) of CTX1B equivalents in fish extract was set at the limit of detection (LOD), being defined as the concentration of CTX1B equivalents inhibiting 20% cell viability (IC20). The LOQ was estimated as 0.0096 ng CTX1B eq. g TE−1 with 23–31% variability between experiments. These values were deemed sufficient even though quantification given at the IC50 (the concentration of CTX1B equivalents inhibiting 50% cell viability) is more accurate with a variability of 17–19% between experiments. Among the 13 fish samp...

Journal ArticleDOI
TL;DR: A methodology for the qualitative and quantitative determination of 34 compounds in slimming preparations (such as dietary supplements or medicinal products) was used for the control of slimming formulations from the market, including over the Internet.
Abstract: The presence on the market of illegal products for slimming purposes or the treatment of overweight is a public health issue. These products may contain illicit chemicals in order to improve their effectiveness. Some of these weight-loss compounds are responsible for adverse events, including fatal outcomes. A general strategy for the analysis of any suspect formulation begins with a large screening for the general search of a wide range of compounds. A methodology for the qualitative and quantitative determination of 34 compounds in slimming preparations (such as dietary supplements or medicinal products) was used for the control of slimming formulations from the market, including over the Internet. The fast liquid chromatography system (ultra-high-pressure liquid chromatography) used a gradient of solvent (phosphate buffer and acetonitrile), a C18 endcapped column and a diode array detector. This system allows dual identification based on retention time and UV spectra. The analytical method is simple, f...

Journal ArticleDOI
TL;DR: Dried fig samples were contaminated with moulds and 94.7% contained one or more mycotoxigenic species, including CPA and fumonisin, found for the first time in dried figs.
Abstract: Mycoflora, the mycotoxigenic properties of moulds, and natural contamination with mycotoxins such as aflatoxins (AFs), cyclopiazonic acid (CPA), fumonisin B1 (FB1) and ochratoxin A (OTA) were investigated in dried figs. Dry fig samples were collected from orchards during the drying stage in the Aegean Region of Turkey. Fungal isolates were identified using morphological, chemical as well as molecular methods. Mycotoxigenic characteristics of moulds were assessed by thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC). Mycotoxins except CPA (by TLC) were determined by HPLC. All the fig samples were contaminated with moulds and 94.7% contained one or more mycotoxigenic species. The most prevalent moulds present in dried figs belong to the Aspergillus section Nigri members, being 93.9% positive for the samples, followed by Fusarium spp., Aspergillus section Flavi and Penicillium spp. On the other hand, Fusarium spp. had the highest count and the number of fumonisin producing Fusa...

Journal Article
TL;DR: The obtained results question the assumptions made by the European Food Safety Authority on the inorganic arsenic level in fish used in the recent EFSA opinion on arsenic in food.
Abstract: The contents of total arsenic and inorganic arsenic were determined in fillet samples of Northeast Artic cod, herring, mackerel, Greenland halibut, tusk, saithe and Atlantic halibut. In total, 923 individual fish samples were analysed. The fish were mostly caught in the open sea off the coast of Norway, from 40 positions. The determination of total arsenic was carried out by inductively coupled plasma mass spectrometry following microwave-assisted wet digestion. The determination of inorganic arsenic was carried out by high-performance liquid chromatography–ICP-MS following microwave-assisted dissolution of the samples. The concentrations found for total arsenic varied greatly between fish species, and ranged from 0.3 to 110 mg kg–¹ wet weight. For inorganic arsenic, the concentrations found were very low (<0.006 mg kg–¹) in all cases. The obtained results question the assumptions made by the European Food Safety Authority (EFSA) on the inorganic arsenic level in fish used in the recent EFSA opinion on arsenic in food.

Journal ArticleDOI
TL;DR: The median estimated daily intake of OTA through the foodstuffs by each age group were below the latest provisional tolerable daily intakes (PTDIs) recommended by the European Food Safety Authority and the Joint FAO/WHO Expert Committee on Food Additives (JECFA) in 2007.
Abstract: Ochratoxin A (OTA) was analysed in composite samples of cereal-based baby foods, beer, breakfast cereals (corn- and rice and wheat-based), loaf bread, peanuts and pistachios. Foodstuffs were collected in hypermarkets and supermarkets from 12 cities in the Spanish region of Catalonia, and composite samples were prepared for analysis involving liquid–liquid extraction, followed by immunoaffinity column clean-up and HPLC with fluorescence detection. Consumption data for the selected foodstuffs were collected by means of a food-frequency questionnaire. The studied population was grouped by age in infants, children, adolescents and adults; and exposure to OTA through the specified foodstuffs, and through wine and coffee, was assessed. Exposure assessment was done through deterministic and probabilistic modelling of the contamination and consumption data. OTA occurrence and mean of positive samples (ng g−1 or ng ml−1, for beer) were the following: 8.7% and 0.233 in baby foods; 88.7% and 0.022 in beer; 2.8% and ...

Journal ArticleDOI
TL;DR: In view of Hg content, the consumption of bay boletes at the regions surveyed at least at a rate up to 2.5 kg per capita weekly in a mushrooming season is safe and will not result in exceeding of currently allowable Hg intake doses.
Abstract: Concentrations of mercury (Hg) were determined in 221 specimens of bay bolete and in 221 samples of corresponding forest topsoil layer (0–10 cm) collected from 18 sites across geographically and industrially diverse regions of Poland in 2000–2008. Mercury concentrations in caps and stipes of bay bolete were strongly correlated (p < 0.0001), whereas the relationship between the Hg concentrations in soil and mushrooms varied depending on the sampling location. The bay bolete showed a lower bioconcentration potential of Hg at sites with elevated soil Hg concentrations and a higher bioconcentration at sites with lower Hg concentrations in soil. In view of Hg content, the consumption of bay boletes (caps or whole mushrooms) at the regions surveyed at least at a rate up to 2.5 kg per capita weekly in a mushrooming season is safe and will not result in exceeding of currently allowable Hg intake doses.

Journal ArticleDOI
TL;DR: A validated method based on European and Brazilian legislation is reported, applicable to the simultaneous determination of chloramphenicol (CAP) and florfenicol (FF) by LC-MS/MS in liquid milk, milk powder and bovine muscle.
Abstract: A validated method based on European and Brazilian legislation is reported. It is applicable to the simultaneous determination of chloramphenicol (CAP) and florfenicol (FF) by LC-MS/MS in liquid milk, milk powder and bovine muscle. The chromatographic analysis is completed in 6 min and the extraction procedure is very simple, involving only one step liquid-extraction with ethyl acetate. Where it proved necessary to include clean-up, an efficient and rapid step using C18-dispersive solid was added. Initially, a complete validation was performed with liquid milk matrix; later the scope was extended to the other matrices through extending the inter-day precision (within laboratory reproducibility) RSD values. An internal standard (d(5)-CAP) was employed for quantitative purposes. The method was shown to have good accuracy and precision for determining CAP residues at the level of 0.3-0.6 g kg(-1) and FF residues at the level of 5-15 µg kg(-1).

Journal ArticleDOI
TL;DR: Among the regulatory toxins in poultry feed, aflatoxin concentrations in 62% of samples were above 20 µg kg−1, demonstrating high prevalence of unsafe levels of aflatoxins in Nigeria.
Abstract: Metabolites of toxigenic fungi and bacteria occur as natural contaminants (e.g. mycotoxins) in feedstuffs making them unsafe to animals. The multi-toxin profiles in 58 commercial poultry feed samples collected from 19 districts in 17 states of Nigeria were determined by LC/ESI–MS/MS with a single extraction step and no clean-up. Sixty-three (56 fungal and seven bacterial) metabolites were detected with concentrations ranging up to 10,200 µg kg-1 in the case of aurofusarin. Fusarium toxins were the most prevalent group of fungal metabolites, whereas valinomycin occurred in more than 50% of the samples. Twelve non-regulatory fungal and seven bacterial metabolites detected and quantified in this study have never been reported previously in naturally contaminated stored grains or finished feed. Among the regulatory toxins in poultry feed, aflatoxin concentrations in 62% of samples were above 20 µg kg−1, demonstrating high prevalence of unsafe levels of aflatoxins in Nigeria. Deoxynivalenol concentrations exce...

Journal ArticleDOI
TL;DR: This study suggests that NS clay also reduces the bioavailability FB1, which is important since AF is a proven dietary risk factor for hepatocellular carcinoma (HCC) in humans and FB1 is suspected to be a dietary risk factors for HCC and oesophageal cancer in humans.
Abstract: Fumonisin B1 (FB1) is often a co-contaminant with aflatoxin (AF) in grains and may enhance AF's carcinogenicity by acting as a cancer promoter. Calcium montmorillonite (i.e. NovaSil, NS) is a possible dietary intervention to help decrease chronic aflatoxin exposure where populations are at risk. Previous studies show that an oral dose of NS clay was able to reduce AF exposure in a Ghanaian population. In vitro analyses from our laboratory indicated that FB1 (like aflatoxin) could also be sorbed onto the surfaces of NS. Hence, our objectives were to evaluate the efficacy of NS clay to reduce urinary FB1 in a rodent model and then in a human population highly exposed to AF. In the rodent model, male Fisher rats were randomly assigned to either FB1 control, FB1 + 2% NS or absolute control group. FB1 alone or with clay was given as a single dose by gavage. For the human trial, participants received NS (1.5 or 3 g day−1) or placebo (1.5 g day−1) for 3 months. Urines from weeks 8 and 10 were collected from the ...

Journal ArticleDOI
TL;DR: Deoxynivalenol contamination was found to increase in most of the study region, with an increase of the original concentrations by up to 3 times, which may inform governmental and industrial risk managers to underpin decision-making and planning processes in north-western Europe.
Abstract: Climate change will affect the development of cereal crops and the occurrence of mycotoxins in these crops, but so far little research has been done on quantifying the expected effects. The aim of this study was to assess climate change impacts on the occurrence of deoxynivalenol in wheat grown in north-western Europe by 2040, considering the combined effects of shifts in wheat phenology and climate. The study used climate model data for the future period of 2031-2050 relative to the baseline period of 1975-1994. A weather generator was used for generating synthetic series of daily weather data for both the baseline and the future periods. Available models for wheat phenology and prediction of deoxynivalenol concentrations in north-western Europe were used. Both models were run for winter wheat and spring wheat, separately. The results showed that both flowering and full maturation of wheat will be earlier in the season because of climate change effects, about 1 to 2 weeks. Deoxynivalenol contamination was found to increase in most of the study region, with an increase of the original concentrations by up to 3 times. The study results may inform governmental and industrial risk managers to underpin decision-making and planning processes in north-western Europe. On the local level, deoxynivalenol contamination should be closely monitored to pick out wheat batches with excess levels at the right time. Using predictive models on a more local scale could be helpful to assist other monitoring measures to safeguard food safety in the wheat supply chain.

Journal ArticleDOI
TL;DR: This is the first biomarker demonstration of DON exposure in pregnant women, and several urinary DON levels were the highest ever recorded in any study.
Abstract: Deoxynivalenol (DON) is a ubiquitous contaminant of cereal crops in temperate regions of the world. It causes growth faltering and immune suppression in animals. Limited information is available on DON exposure in UK subpopulations. The objective of this study was to provide DON exposure assessment in a subset of pregnant women scheduled for an elective caesarean in a large multi-ethnic mother/infant birth cohort from Bradford, UK. Women aged 16–44 years (n = 85) provided a urine sample for DON analysis in the last trimester of pregnancy, and concurrently completed a food-frequency questionnaire (FFQ). The urinary DON biomarker was detected in all measured samples (geometric mean (GM) = 10.3 ng DON mg−1 creatinine, range = 0.5−116.7 ng mg−1). Levels were higher in women classified as South Asian in origin (GM: 15.2 ng mg−1; 95% CI = 10.7−21.5 ng mg−1) compared with non-South Asians (GM = 8.6 ng mg−1; 95% CI = 6.6−11.8 ng mg−1), p = 0.02). Estimated DON intake from FFQ data and typical levels of DON contam...