Fumonisin intake of the German consumer.

In order to calculate the dietary fumonisin intake of the German consumer, a large survey was carried out on a variety of potentially contaminated products in the period between December 1998 and July 2001. A total of 1960 food samples comprising all known relevant groups of products were analysed for fumonisins. Furthermore, 272 of these samples were also analysed for hydrolysed fumonisins (HFB). For routine analysis enzyme immunoassay was used, confirmatory and control analyses were performed using HPLC-FLD after precolumn derivatisation, or by LC-MS/MS. Daily intake of fumonisins was calculated by combining fumonisin contamination data obtained in this study with available food consumption data for Germany. In a "mean case" scenario, median fumonisin levels in foods and mean food intake values were used. To generate a "bad case" scenario, the 90(th) percentile of fumonisin levels in foods and mean food intake values were combined. The overall daily fumonisin intake by the German consumer was 1.1 µg in the "mean case" scenario, and 21 µg in the "bad case" scenario. It was concluded that in general there is no increased risk for the German consumer in aspects of exceeding the recommended tolerable daily intake of fumonisins (2 µg/kg body weight). However, certain products (and certain brands of products) were repeatedly found to contain elevated fumonisin levels, which in a "worst case" scenario ("high" food intake of maize-based products) could pose a potential risk for the consumer, in particular concerning foods for infants and young children. High fumonisin levels were found in infant foods in 1999, but contamination levels decreased strongly in the following years. HFBs (mostly HFB1) were frequently found in processed cereals such as corn flakes, but in relatively low concentrations. According to our findings, the new European Union maximum levels for fumonisins are suitable to eliminate peak contamination levels of fumonisins in foods, but would lead to a regular excess of the TDI for infants and young children if these maximum levels would indeed be exhausted.

Determination of ergot alkaloids in rye and rye flour.

An effective and timesaving analytical method was developed for the determination of 12 ergot alkaloids (ergometrine, ergotamine, ergocristine, α-ergokryptine, ergosine, ergocornine, and their respective -inine isomers) in rye and rye flour. Samples were extracted with dichloromethane/ethyl acetate/methanol/aqueous ammonia (25%) (50/25/5/1, v/v/v/v), and extracts were purified using a basic alumina column. The eluate was dried in the nitrogen stream and redissolved in acetonitrile/ ammonia carbamate-buffer (0.2 g/1), (1/1, v/v), and injected into an HPLC-FLD system (λEx 330 nm, λEm 415 nm), using the same mixture as mobile phase and a Phenyl-Hexyl column. Detection limits for the individual compounds ranged from 0.01 µg/kg to 0.5 µg/kg. In sample material spiked with a mixture of these compounds at two different levels (13 µg/kg and 27 µg/kg per compound), mean (n=5) recoveries were at 101% (sr 6.4%) and 89% (sr 3.1%), respectively.

Acrylamide-occurrence in mixed concentrate feed for dairy cows and carry-over into milk.

During the preparation of cooked foods acrylamide is formed from asparagine and reducing sugars at high temperatures. By-products of oil, starch and sugar production, which may be found in animal feed, partially result from processing steps using heat treatment that are similarly likely to form acrylamide. Possibly, pelletizing during the processing of mixed concentrates may also be involved in acrylamide formation. Thus the occurrence of acrylamide in animal feed and the potential for carry-over into animal products should be tested. Independently of the feed matrix, 1.5 g per day of acrylamide was fed to a cow for ten days resulting in a mean concentration of 175 microg/kg of acrylamide in the milk. From the data obtained the mean carry-over was found to be 0.24%, and a mean half-life time of 2.8 h was estimated. This means acrylamide was rapidly transformed in the cow. The acrylamide concentrations in three commercial mixed concentrates were respectively 180, 145 and 140 microg/kg feed. To test the possible effect of pelletizing, the peripheral zones were separately analysed. No difference in concentration was observed. Based on the carry-over rate estimated in this study, a maximum concentration of approx. 0.2 microg/kg of acrylamide would be expected in milk from cows fed with such feeds.

[Determination of zearalenone in edible oils with SEC and LC-ESI-MS/MS]. / Bestimmung von Zearalenon in Speiseölen mit GPC und LC-ESI-MS/MS.

A new method for the determination of zearalenone in edible oils with size exclusion chromatography (SEC) followed by LC-MS/MS as well as HPLC-FLD was developed and validated. By using the LC-MS/MS determination no further clean up step is necessary after the SEC. The correlation coefficient of 0.999 for the two detection systems is acceptable. In this research 77 edible oils were analyzed. The mean average value of 38 corn germ oils was 169 µg/kg, the maximum value amounted up to 921 µg/kg.

[Zearalenone in food]. / Zearalenon in Lebensmitteln.

The research project "Methods of Analysis and occurrence of important Fusarium toxins (deoxynivalenol and zearalenone) as well as the intake of these toxins by the German consumer" supported by the Federal Ministry of Consumer Protection, Food and Agriculture (BMVEL) is processed by the institutions mentioned above. This work represents a comprehensive summary of the contamination of food by zearalenone (ZEA).

[Deoxynivalenol in food]. / 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.

[Not Available]. / Bestimmung von deoxynivalenol mittels LC - MS/MS (Tandem Massenspektrometrie).

A sensitive and selective method using high-performance liquid chromatography in combination with atmospheric pressure chemical ionization tandem mass spetrometry (LC-APCI-MS/MS) has been developed for the determination of Deoxynivalenol (DON) in trace levels. The extract was purified with a MultiSep™ column followed by the Vicam™ DON immunoaffinity column. Quantification is based on an external standard method using positive Multiple Reaction Monitoring (MRM). The limit of detection was 5 µg/kg with a signal to noise ratio of 3:1.

[Not Available]. / Bestimmung von Fumonisinen in komplexen Lebensmittelmatrices mittels Accelerated Solvent Extraktion (ASE).

Accelerated solvent extraction (ASE) is an alternative sample extraction procedure for fumonisins in corn and corn products. ASE gave results comparable to that of a draft CEN method, but required less extraction time. Furthermore, ASE gave significantly higher quantitative values than another method reported for extraction of fumonisins (Trucksess et al., 1995).