Bestimmung von Zearalenon in Speiseölen mit GPC und LC-ESI-MS/MS

Kappenstein, Oliver; Klaffke, H.; Mehlitz, Irena; Tiebach, R.; Weber, Rudolf; Lepschy, J.; Wittkowski, R.

doi:10.1007/bf02954804

Cited by 19 publications

(12 citation statements)

References 4 publications

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“…Determination of zearalenone in maize oil was carried out by extraction and clean-up with gel permeation chromatography, followed by HPLC/tandem mass spectrometry (Biopharm 2009;Kappenstein et al 2005).…”

Section: Zearalenonementioning

confidence: 99%

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

Reinhold

Reinhardt

2011

Mycotox Res

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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.

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Section: Zearalenonementioning

confidence: 99%

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

Reinhold

Reinhardt

2011

Mycotox Res

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“…When we searched for alternatives to the GPC procedure (Kappenstein et al 2005), the multi-method according to Kocher (2006), which allows oils to be examined for zearalenone, as well as, in particular, ochratoxin A, trichothecenes, and aflatoxins, in a relatively short period of time via the so-called echo method, was an attractive option. However, the alkaline extraction medium over a relatively long time period of 30 min causes the lactone ring to open, thereby depriving the zearalenone molecule of its fluorescent properties, rendering it unavailable for measurement by fluorescence detection.…”

Section: Resultsmentioning

confidence: 99%

“…In three separate experiments, the effect of various acid conditions (i.e., inadvertent addition of excess hydrochloric acid to the alkaline extract) on the fluorescence determination of zearalenone was studied (Table 3). In selected samples, a comparison of the GPC sample preparation as described by Kappenstein et al (2005) and the acid-base treatment described in this study was performed ( Table 4). Chromatograms of a zearalenone standard solution (100 pg/µl), of a blank rapeseed oil sample contaminated with zearalenone at 27 µg/kg, and of a naturally contaminated maize oil sample contaminated with zearalenone at 212 µg/kg (are shown in Fig.…”

Section: In-house Validationmentioning

confidence: 99%

“…The dietary intake of adults and children was estimated to be 5.3-14.5% and 3-27.5%, respectively, of the temporary TDI (tolerable daily intake) of 0.2 µg/kg body weight/day. The occurrence of zearalenone in edible oils using gel permeation chromatography (GPC) for extraction and LC-MS/MS for detection was first reported by Kappenstein et al at the 26th mycotoxin workshop 2004 in Herrsching, Germany (Kappenstein et al 2005) A procedure for analysis of zearalenone in grains, grain products, and baby food is currently being normalized in Europe as part of the CEN TC 275 WG5 Biotoxins (MacDonald et al 2005;Arranz et al 2007). But this procedure is not suitable for determining zearalenone in edible oils.…”

Section: Introductionmentioning

confidence: 97%

“…Comparison of results for zearalenone in edible oil after gel permeation chromatographic cleanup (GPC method;Kappenstein et al 2005) and after acid-base-treatment as developed in this study (determination byHPLC-FLD) …”

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confidence: 99%

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Rapid determination of zearalenone in edible oils by HPLC with fluorescence detection

2009

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A fast, cost-efficient, sensitive and accurate assay method for zearalenone in edible oils is described, as an alternative to gel permeation chromatography (GPC). Oil samples were extracted with an alkaline mixture of methanol and water (methanol +10 g/l aqueous ammonium carbaminate solution, pH 9; 9 + 1, v+v). The pH of the extract was neutralized with hydrochloric acid and then concentrated to dryness. The residue was dissolved with HPLC solvent, and zearalenone was determined by high-performance liquid chromatography with fluorometric detection (HPLC-FLD). The method was successfully validated for two matrices, maize oil and rapeseed oil. The recovery rate was 87%, and the coefficient of variation was 2.8% in a rapeseed oil sample contaminated with 27 µg zearalenone/kg. At a signal-to-noise ratio of 3:1, the method detection limit was 10 µg/kg, which was considered to be adequate in view of the present European Union maximum level of 400 µg/kg.

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