Deoxynivalenol contents in foodstuffs of organical and conventional production

Samples of wheat flour, bread, noodles, rice, corn and corn based foods as well as oats and oats based foods of conventional and organical production were analysed for trichothecene toxins. In wheat flour, bread and noodels the median deoxynivalenol (DON) contents were lower in ecological than in conventional products with significant differences for what flour and bread. To estimate toxin uptake of the consumer a corrected mean of DON concentration was calculated, which was lower in wheat flour and bread for ecological than for conventional products. In noodles the corrected mean of organical products was higher than that of conventional ones.     

Occurrence of<Emphasis Type="Italic">Fusarium</Emphasis> toxins in the 1999’s harvest

Continuing the monitoring ofFusarium toxins in cereals, we investigated 245 samples of wheat, barley, triticale and oats in 1999. 84 samples out of 100 analysed forFusarium could be found to be infected. The most prominentFusarium species detected whereF. avenaceum, F. poae, F. detected whereF. avenaceum, F. poae, F. graminearum, andF. sporotrichoides. The level of mycotoxin contamination of the samples varied depending on their origins and was in general very low in comparison with the result obtained in samples of the previous year. There where only some wheat samples with deoxynivalenol (DON) concentrations beyond existing advisory levels. The average DON concentration of all samples was 0.35 mg/kg with a median of 0.007 mg/kg. 3-Acetyldeoxynivalenol and zearalenone (ZEA) could only be detected at minor concentrations (below 0.1 and 0.05 mg/kg, respectively) in less than 10% of the samples. The analysis of commercial cereal flour reflects this situation. Flour bought in the first quarter of 1999, which was suspected to contain a high portion of the 1998 harvest, was contaminated by DON to a higher extent than those purchased in 2000. The average DON concentration in the flour samples of 1999 and 2000 was 0.35 mg/kg and 0.23 mg/kg, respectively. Although the general mycotoxin level in the 1999 harvest was lower as in 1998 there were some highly contaminated samples that had mainly been grown in fields with either maize or other cereals as previous crop and reduced tillage. The combination of maize as previous crop and non-tillage could be stated as most unsuitable, which promotes enhanced mycotoxin contamination, and should therefore be avoided.     

Immunochemical assessment of mycotoxins in 1989 grain foods: evidence for deoxynivalenol (vomitoxin) contamination

To assess the potential for mycotoxin contamination of the human food supply following the 1988 U.S. drought, 92 grain food samples were purchased from retail outlets in the summer of 1989 and surveyed for aflatoxin B1, zearalenone, and deoxynivalenol (DON [vomitoxin]) by monoclonal antibody-based competitive enzyme-linked immunosorbent assay (ELISA). Only one sample (buckwheat flour) was found to contain aflatoxin B1 (12 ng/g), whereas zearalenone was found in 26% of the samples at a mean concentration of 19 ng/g. In contrast, the DON ELISA was positive in 50% of the samples at a detection level of 1.0 micrograms/g. Between 63 and 88% of corn cereals, wheat flour/muffin mixes, rice cereals, and corn meal/muffin mixes yielded positive results for DON, whereas 25 to 50% of oat cereals, wheat- and oat-based cookies/crackers, corn chips, popcorn, and mixed-grain cereals were positive for DON. The mean DON content of the positive samples was 4.0 micrograms/g, and the minimum and maximum levels were 1.2 and 19 micrograms/g, respectively. When positive ELISA samples were also analyzed by high-performance liquid chromatography, a strong correlation between the two methods was found. The presence of DON in the two highest samples, corn meal and mixed-grain cereal, which contained 19 and 16 micrograms/g, respectively, was quantitatively confirmed by gas chromatography-mass spectrometry. The results indicated that DON was present in 1989 retail food products at concentrations that exceeded those found in previous market surveys and that have been experimentally associated with impaired animal health.     

Immunochemical assessment of mycotoxins in 1989 grain foods: evidence for deoxynivalenol (vomitoxin) contamination.

To assess the potential for mycotoxin contamination of the human food supply following the 1988 U.S. drought, 92 grain food samples were purchased from retail outlets in the summer of 1989 and surveyed for aflatoxin B1, zearalenone, and deoxynivalenol (DON [vomitoxin]) by monoclonal antibody-based competitive enzyme-linked immunosorbent assay (ELISA). Only one sample (buckwheat flour) was found to contain aflatoxin B1 (12 ng/g), whereas zearalenone was found in 26% of the samples at a mean concentration of 19 ng/g. In contrast, the DON ELISA was positive in 50% of the samples at a detection level of 1.0 micrograms/g. Between 63 and 88% of corn cereals, wheat flour/muffin mixes, rice cereals, and corn meal/muffin mixes yielded positive results for DON, whereas 25 to 50% of oat cereals, wheat- and oat-based cookies/crackers, corn chips, popcorn, and mixed-grain cereals were positive for DON. The mean DON content of the positive samples was 4.0 micrograms/g, and the minimum and maximum levels were 1.2 and 19 micrograms/g, respectively. When positive ELISA samples were also analyzed by high-performance liquid chromatography, a strong correlation between the two methods was found. The presence of DON in the two highest samples, corn meal and mixed-grain cereal, which contained 19 and 16 micrograms/g, respectively, was quantitatively confirmed by gas chromatography-mass spectrometry. The results indicated that DON was present in 1989 retail food products at concentrations that exceeded those found in previous market surveys and that have been experimentally associated with impaired animal health.     

Deoxynivalenol in lebensmitteln: Ergebnisse einer Pilotstudie

Cereal food products (n=333) were purchased in retail stores from Germany in 2001 and analysed for deoxynivalenol (DON), either by enzyme immunoassay or by HPLC after immunoaffinity chromatographic cleanup. Detection limits were dependent of the sample matrix and varied from 20–100 μg/kg. The overall DON incidence was 53%, with mean and median levels for positives of 251 μg/kg and 142 μg/kg, respectively. The contamination with DON (mean/median value, μg/kg) as found for bread (90/87), wheat flour (161/124), and noodles (472/297) indicate that the levels of DON in cereal foods were significant in view of the tolerable daily intake (1 μg/kg body weight) as established by the European Union scientific committee on food.     

Preliminary exposure assessment of deoxynivalenol and patulin in South Africa

Deoxynivalenol (DON) and patulin (PAT) are mycotoxins widely regulated internationally. DON is frequently found in cereals, whereas PAT is commonly found in apple juices. A survey of South African commercial products was conducted on DON levels in maize meal and wheat flours, and on PAT levels in apple juices. DON levels in 23 wheat flour samples (mean of 16 positives, 29 μg/kg) were equal to or below 100 μg/kg and in wheat consumers contributed 6–13% of the provisional maximum tolerable daily intake (PMTDI; 1 μg/kg body weight per day) for DON set by the Joint FAO/WHO Expert Committee on Food Additives (JECFA). Sixteen of 18 maize meal samples were contaminated, with a mean for positive samples of 294 μg/kg, and the probable daily intakes ranged from 3.67 μg/kg body weight per day in rural infants to 1.39 μg/kg body weight per day in urban adults. PAT levels in 20 of 30 apple-juice samples were below the detection level of 10 μg/l. Mean of positive samples was 210 μg/l, with three samples exceeding the South African legal limit of 50 μg/l and the highest level (1,650 μg/l) showing the possibility of a brief but high exposure of 37 μg/kg body weight per day (or 9,250% of the JECFA PMTDI of 0.4 μg/kg body weight per day) in young children.     

Deoxynivalenol in Mehlproben des Jahres 1999 aus dem Einzelhandel

To study the levels of deoxynivalenol (DON) in retail cereal products, wheat and rye samples were purchased in 1999 from supermarkets and “organic food” shops in Munich, Germany. DON was analysed by an enzyme immunoassay (EIA), 78 of these samples were additionally analysed by HPLC. The following contamination rates (%) and mean DON levels were found: wheat flour type 405 (n=42): 71%, 200 µg/kg; flour type 550 (n=9): 33%, 410 µg/kg; flour type 1050 (n=11): 91%, 370 µg/kg; bread-baking wheat premixes (n=14): 79%, 210 µg/kg; whole grain flour (n=20): 65%, 300 µg/kg; whole grain wheat (n=8): 75%, 280 µg/kg, wheat bran (n=20): 85%, 830 µg/kg; rye flour and grits (n=7): 29%, 120 µg/kg. HPLC confirmed the results obtained by EIA. Further analysis of 16 wheat flour (405) samples in May 2000 showed a similar frequency (69%) and mean DON level (270 µg/kg) as for samples from 1999. It is concluded that with DON levels in wheat for human consumption ranging from 200–400 µg/kg, the intake of DON has to be taken seriously in the light of the temporary tolerable daily intake of 1 µg DON per kg body weight as proposed within the European Union.     

Mycotoxins in foods in Lower Saxony (Germany): results of official control analyses performed in 2009

In this presentation, the mycotoxin levels—as analysed by the analytical centre for mycotoxin surveillance of the state food laboratory (LAVES Braunschweig)—for approximately 500 food samples are reported. The samples were collected in the year 2009 at retail in the German federal state of Lower Saxony. Aflatoxin and ochratoxin A were analysed in dried fruits, spices, cereals and tree nuts. Ochratoxin A was detected in all samples of dried vine fruits, at levels up to 8.1 μg/kg. Aflatoxins and ochratoxin A were also found in nutmeg and curry powder: the maximum regulatory levels for aflatoxins were exceeded in 25% of the nutmeg samples. Nearly all samples of basmati rice contained aflatoxins, although at levels below the maximum regulatory level in all but one sample. Aflatoxins were also detected in about 50% of hazelnut samples, in 20% of the samples the maximum levels was exceeded (maximum 23.2 μg/kg). In contrast, aflatoxin contents in pistachios were surprisingly low. Fusarium toxins were analysed in cereals and cereal products such as flour, bread, and pasta. Deoxynivalenol (DON) was the predominant toxin found in these samples: DON was found in about 40% of the samples, although the maximum levels were not exceeded (max. 418 μg/kg). Fumonisins (FBs) and zearalenone (ZEA) were specifically analysed in maize products (snacks, flour and oil). Most of these samples (80%) were positive, but at levels not exceeding the maximum levels. Maximum levels were 98 μg/kg (ZEA) and 577 μg/kg (sum of FB₁ and FB₂). Ergot alkaloids (six major alkaloids) were analysed in rye flour, and approximately 50% were positive. The highest concentration of ergot alkaloids was 1,063 μg/kg; the predominant alkaloids were ergotamine and ergocristine. In conclusion, the results indicate that continuous and efficient control measures for mycotoxins in a wide range of critical foods are necessary to ensure compliance with maximum levels. Although the mycotoxin levels in the vast majority of samples were below maximum levels, year-to-year variation and changes in the production of relevant commodities may result in a different picture in the future.     

A survey of Fusarium toxins in cereal-based foods marketed in an area of southwest Germany

A total of 237 commercially available samples of cereal-based foods including bread and related products, noodles, breakfast cereals, baby and infant foods, rice and other foods were randomly collected in southwest Germany during the first six months of 1998. The trichothecenes deoxynivalenol (DON), 3-and 15-acetyl-deoxynivalenol (3-,15-ADON), nivalenol (NIV), fusarenon-X (FUS-X), T-2 toxin (T-2) and HT-2 toxin (HT-2) were determined by gaschromatography/mass spectrometry following clean-up by a two stage solid-phase extraction. Detection limits ranged between 2 and 12 g/kg. Based on all samples, the incidence of DON, HT-2, T-2, 3-ADON,15-ADON, and NIV was at 71, 18, 4, 4, 4 and 2%, respectively; the average contents in positive samples were at 103, 16, 14, 17, 24 and 109 g/kg,respectively. Fus-X was not detected in any sample. A lower (P < 0.05) DON content was found in baby and infant foods as well as in cookies and cakes compared to bread. Overall, based on the incidence and level of all six toxins, the degree of contamination was lowest in baby and infant foods. Foods produced from either white or whole grain flour did not differ (P > 0.05) with regard to the incidence and level of DON. In foods produced from cereals of organic production both the incidence and median content of DON was lower compared to conventional production. Zearalenone, - and -zearalenol were determined by high performance liquid chromatography in 20 selected samples, mostly baby and infant foods. These toxins were not present in excess of the detection limit in any sample.This revised version was published online in October 2005 with corrections to the Cover Date.     

Deoxynivalenol in Lebensmitteln

Within a joint research project entitled “Analysis and occurrence of importantFusarium toxins (deoxynivalenol and zearalenone) and dietary intake of these toxins by the German consumer”, supported by the German Federal Ministry of Consumer Protection, Food and Agriculture (BMVEL), representative analytical data are generated on the contamination level of foods withFusarium mycotoxins. This paper gives a comprehensive summary concerning the contamination of foods from the German market with deoxynivalenol (DON) in the period from August 2001 to April 2004. More than 4700 food samples (mostly cereals and cereal-containing foods) were purchased from food shops in Germany and analysed for DON by enzyme immunoassay, HPLC, and LC-MS/MS, respectively. All analytical methods were validated through intra- and interlaboratory studies and gave mean recoveries of >80% for each matrix. Although DON was detected with high frequency in all cerealcontaining samples, the mean and median levels were in most products well below the recently established maximum permitted limits in Germany.     

Determination of deoxynivalenol in cereals by immunoaffinity clean-up and ultra-high performance liquid chromatography tandem mass spectrometry

An immunoaffinity column (IAC) was prepared with a new deoxynivalenol (DON) monoclonal antibody and used as a clean-up tool before ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) analysis of DON in cereals. The developed IAC clean-up method showed high recoveries for DON. They ranged from 61% to 103% in wheat, rice, and millet with intra-day and inter-day variations below 19% and 17%, respectively. The column capacity was 2.86μg DON per mL of gel, and it maintained above 0.68μg/mL of gel after 10 cycles of usage at 2 days intervals. The limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 0.8μg/kg, respectively. Twenty-one out of 40 analyzed commercial cereal samples were positive at DON concentrations from 7 to 534μg/kg.     

Occurrence of different trichothecenes and deoxynivalenol-3-β-d-glucoside in naturally and artificially contaminated Danish cereal grains and whole maize plants

Fusarium mycotoxins such as deoxynivalenol (DON) can occur in cereals conjugated to glucose and probably also to other sugars. These conjugates, which are often referred to as ??masked mycotoxins??, will not be detected with routine analytical techniques. Furthermore, it is suspected that the parent toxin may again be released after hydrolysis in the digestive tracts of animals and humans. Today, our knowledge of the occurrence of these compounds in cereal grains is limited. In this paper, a LC-MS/MS method for the simultaneous determination of DON, deoxynivalenol-3-??-d-glucoside (DON-3-glucoside), 3 acetyl-DON, nivalenol, fusarenon-X, diacetoxyscirpenol, HT-2 toxin, and T-2 toxin in naturally (n?=?48) and artificially (n?=?30) contaminated cereal grains (wheat, barley, oat, rye triticale) is reported. The method has also been applied to whole fresh maize plant intended for production of maize silage (n?=?10). The samples were collected from the harvest years 2006?C2010, The results show that DON-3-glucoside and DON co-occurred in cereal grains and, especially in several of the highly contaminated samples, the concentration of the glucoside can be relatively high, corresponding to over 37?% of the DON concentration. The DON-3-glucoside levels in both the naturally and in the artificially grain inoculated with Fusarium were second only to DON, and were generally higher than those of the other tested trichothecenes, which were found at low concentrations in most samples, in many cases even below the detection limit of the method. This argues for the importance of taking DON-3-glucoside into account in the ongoing discussion within the European Community concerning exposure re-evaluations for setting changed values for the tolerable intake for DON. Our results indicate that, in the naturally contaminated grains and in the Fusarium infested cereal grains (winter and spring wheat, oat, triticale), the concentration level of DON-3-glucoside is positively correlated to the DON content. When the DON concentration is high, then the content of DON-3-glucoside will most probably also be high and vice versa.     

Effekte von Be- und Verarbeitung auf die Deoxynivalenol- und Zearalenongehalte in Getreide und Getreideprodukten

Since national limits have been introduced for the content of DON and ZEA in cereals and cereal products designated for human consumption, it is highly important to understand how these toxins are distributed during sorting, cleaning and further processing to bakery products and pasta. Cereals from several crops were analysed before and after sorting and cleaning. After milling, flours, breads, semolinas, pastas and others were analysed. The results show that that the distribution of DON and ZEA was different. ZEA was more effectively removed than DON. The efficacy of the various processes varied markedly from one lot to the other.     

Mycotoxins in organic and conventional cereals and cereal products grown and marketed in Croatia

In this study, the levels of aflatoxin B₁ (AFB₁), ochratoxin A (OTA), zearalenone (ZEN), deoxynivalenol (DON) and fumonisins (FUM) in unprocessed cereals (n = 189) and cereal-based products (n = 61) were determined using validated ELISA methods. All samples originated from either conventional or organic production corresponded to the 2015 harvest in Croatia. Based on the mean mycotoxin concentrations, the risk for the consumer to exceed the tolerable daily intake (TDI) for these toxins by the consumption of both types of cereals and cereal-based products was assessed. Mycotoxin contamination of organic cereals and organic cereal-based products was not significantly different (p > 0.05). Given that the exposure assessment resulted in a small fraction of the TDI (maximum: DON, 12% of TDI), the levels of the investigated mycotoxins in both types of cereals and cereal-based products from the 2015 harvest did not pose a human health hazard.     

Fusarium toxins in different food samples

Samples of wheat for human nutrition, wheat flour, bread and noodles were analysed for different trichothecenes and partly for zearalenone (ZEA). The toxin contents for deoxynivalenol (DON) and ZEA were compared with the maximum tolerated levels recently discussed for foodstuffs in Germany. The limits for DON were exceeded in 20, 15, 5 and 9% of the samples of wheat, wheat flour, bread and noodles respectively, the limits for ZEA in 4 and 0% for wheat and wheat flour respectively.     

Wholemeal versus wholegrain breads: proportion of whole or cracked grain and the glycaemic response.

STUDY OBJECTIVE--To determine the effect on the glycaemic response to bread of the ratio of whole cereal grains to milled flour. DESIGN--Randomised assignment of groups of diabetic volunteers to test and control meals, taken after an overnight fast. Test foods were also analysed for in vitro digestion with human saliva. SETTING--Tertiary care centre. PATIENTS--Groups of six drawn from pool of 16 volunteers with diabetes mellitus (11 men, five women; mean age 64 (SE 3); 10 taking insulin, five taking oral agents, one controlled by diet; other characteristics comparable). INTERVENTIONS--All patients took standard white bread control meals on three occasions spanning the study and on different mornings took test meals containing varying ratios of whole cereal grains (barley or cracked wheat) to milled flour (75:25, 50:50, 0:100). All meals contained 50 g available carbohydrate and were eaten in 15 minutes. Capillary blood samples were taken for determination of glucose concentrations every 30 minutes for three hours. END POINT--Glycaemic index of foods (= increase in area under blood glucose concentration curve for test food divided by increase in area under curve for white bread control X 100). MEASUREMENTS AND MAIN RESULTS--Significant trend to lower glycaemic index with increasing proportion of whole cereal grains in test bread (p less than 0.05) and lower in vitro digestibility (p less than 0.001). Breads containing up to 75% whole grain were considered palatable. CONCLUSIONS--Breads containing a high proportion of whole cereal grains may be useful in reducing the postprandial blood glucose profile in diabetics because they are more slowly digested. These breads should be called "wholegrain" in distinction to "wholemeal" breads made from milled flour.     

A study of the suitability of gas chromatography-electron capture detection for the analysis of deoxynivalenol in cereals

A gas chromatographic-electron capture detection (GC-ECD) method for the analysis of deoxynivalenol (DON) in cereals was investigated. The sample was extracted with a mixture of acetonitrile-water and purified with a MycoSep #225 column. The silylation was performed with Tri-Sil-TBT reagent, followed by dilution with hexane and a washing step with buffer. By using Tri-Sil-TBT reagent no double peaks were observed for DON in the gas chromatograms, in comparison with two other silylation reagents TMSI and Tri-Sil-Z. The use of trichothecolone (TRI) as an internal standard for DON was studied in order to indicate possible problems in the derivatisation reaction. TRI proved to be a relatively good internal standard for DON in cereal samples, as well as 1,1-bis-(4-chlorophenyl)-2,2-dichloroethylene (DDE), which was used as a GC standard for ensuring the function of GC-ECD. During the study, a matrix effect was clearly observed between the cereal matrix-assisted calibration curve and the calibration curve prepared without cereal matrix. The results of spiked and reference material samples, quantified with the calibration curve prepared without and with matrix, demonstrated that the matrix affects the results. However, after recovery correction the results were comparable. The validation results demonstrated that the GC-ECD method for DON analysis in cereals is sufficiently reliable.     

Gesetzliche Regelungen für Mykotoxine in Lebensmitteln (Official Regulations on Mycotoxins in Food)

When establishing maximum limits, in addition to issues relating to preventive consumer protection and toxicological data on risk assessment, sampling procedures and methods of analysis, as well as economic and political aspects have to be considered. Therefore, various and diverse organizations tend to be involved in the process of establishing maximum limits. Specifically, the following are responsible for the toxicological evaluation of the substances in question: International Programme on Chemical Safety (IPCS), International Agency of Research on Cancer (IARC), Joint FAO/WHO Expert Committee on Food Additives (JECFA), and, within the Commission of the European Communities, the Scientific Committee for Food (SCF). The interests of world-wide trade are looked after by the Codex Alimentarius Commission, the Codex Committee of Food Additives and Contaminants, and the World Trade Organisation, WTO. On the basis of Commission Regulation (EC) no. 315/93, in 2001 the EU has adopted Commission Regulation (EC) no. 466/2001 on contaminants establishing maximum limits for nitrates, heavy metals, 3-monochlor-propan-1,2-diol, and aflatoxins in foods (peanuts, nuts, dried fruits, cereal/cereal products). In February 2002, this Regulation has been completed by Regulation (EC) no. 257/2002 (aflatoxins in cereals), and in March 2002 by Regulation (EC) no. 472/2002 (aflatoxins in spices and ochratoxin A in cereals and dried grapes). Reference is made to other mycotoxins the levels of which in certain foods should be the subject of future regulations.     

Monitoring of fusarium toxins in cereals and feed-stuffs from thuringia (1998 - 2001)

From 1998 to 2001 a total of about 1172 conventionally and organically produced samples of wheat, rye, barley and triticale were examined for the presence of deoxynivalenol (DON) and zearalenone (ZON). Furthermore, feedstuffs for pigs were included in the monitoring of Fusarium toxins. DON and ZON analyses were performed using ELISA or HPLC. The incidences and levels of toxins varied from year to year. Overall contamination levels were highest in wheat and triticale, followed by rye and barley. The highest DON contaminations were found in 1998. The probes of the years 1999-2001 showed lower incidences of Fusarium toxins. The second examined mycotoxin ZON was detected at lower levels in cereals. Similar results were observed in the monitoring of feedstuffs.