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Simultaneous determination of major type A and B trichothecenes, zearalenone and certain modified metabolites in Finnish cereal grains with a novel liquid chromatography-tandem mass spectrometric method.

Nathanail AV, Syvähuoko J, Malachová A, Jestoi M, Varga E, Michlmayr H, Adam G, Sieviläinen E, Berthiller F, Peltonen K - Anal Bioanal Chem (2015)

Bottom Line: Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively.Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing.All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time.

View Article: PubMed Central - PubMed

Affiliation: Chemistry and Toxicology Unit, Research and Laboratory Department, Finnish Food Safety Authority (Evira), Mustialankatu 3, 00790, Helsinki, Finland, alexis.nathanail@helsinki.fi.

ABSTRACT
A reliable and sensitive liquid chromatography-tandem mass spectrometric method was developed for the simultaneous quantitative determination in cereals of the Fusarium mycotoxins HT-2 toxin, T-2 toxin, deoxynivalenol, nivalenol and zearalenone, as well as the modified metabolites 3-acetyl-deoxynivalenol, α-zearalenol, β-zearalenol, deoxynivalenol-3-glucoside, HT-2-3-glucoside, nivalenol-3-glucoside, zearalenone-14-glucoside, zearalenone-14-sulphate, zearalenone-16-glucoside, α-zearalenol-14-glucoside and β-zearalenol-14-glucoside. The 'dilute and shoot' approach was used for sample preparation after extraction with acetonitrile:water:acetic acid (79:20:1, v/v/v). Separation was carried out using reversed-phase liquid chromatography, and detection was performed using tandem mass spectrometry in the selected reaction monitoring mode. The method was in-house validated according to performance characteristics, established in Commission Regulation EC No 401/2006 and Commission Decision EC No 657/2002, prior to its application in a nationwide survey for the analysis of barley, oat and wheat samples (n = 95) harvested in Finland during 2013. Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively. Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing. All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time.

No MeSH data available.


Related in: MedlinePlus

Overview of the Fusarium mycotoxins and modified mycotoxins detected in Finnish cereal grains in 2013 (n = 95)
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Fig4: Overview of the Fusarium mycotoxins and modified mycotoxins detected in Finnish cereal grains in 2013 (n = 95)

Mentions: The developed and validated LC-MS/MS method was applied for the analysis of 95 cereal grain samples from Finland harvested during 2013, and the results are summarised in Table 4. Figure 4 presents an overview of the detected mycotoxins and modified mycotoxins in barley, oats and wheat. The results of our survey revealed considerable variation between different commodities. The highest contamination of the studied mycotoxins was observed in oats, followed by wheat and barley. The most frequently detected native mycotoxin was DON (incidence 93 % of the samples analysed), followed by NIV (63 %) and HT2 (57 %). DON was also found at the highest concentrations, and particularly in wheat and oats, with 32 % of the analysed oats exceeding the legislative ML of 1750 μg/kg set for DON regarding unprocessed oats placed on the market for first-stage processing [27]. For wheat, the percentage of samples exceeding the ML (1250 μg/kg) was 23 %, whereas no barley sample exceeded the same level. 3Ac-DON (55 %) was only found at increased levels in oats, in samples also showing high concentrations of DON. One wheat and one oat sample also exceeded the ML set for ZEN (100 μg/kg), and both were also highly contaminated with DON (1660 and 23,800 μg/kg, respectively). Such DON levels are unusually high compared to those of previous years based on quantitative results from the Finnish grain quality monitoring programme (1999–2009) [9]. Only minor amounts of HT2 and T2 were detected in barley and wheat. In contrast, the prevalence of these toxins in oats was significantly more pronounced. Nonetheless, only one sample exceeded the indicative value for the sum of these toxins (1000 μg/kg) in Recommendation 2013/165/EU for unprocessed oats [28]. NIV contamination was relatively low in barley and wheat samples in comparison to the levels found in oats, with a mean concentration of 635 μg/kg that can be attributed to four very highly contaminated samples (>1400 μg/kg).Table 4


Simultaneous determination of major type A and B trichothecenes, zearalenone and certain modified metabolites in Finnish cereal grains with a novel liquid chromatography-tandem mass spectrometric method.

Nathanail AV, Syvähuoko J, Malachová A, Jestoi M, Varga E, Michlmayr H, Adam G, Sieviläinen E, Berthiller F, Peltonen K - Anal Bioanal Chem (2015)

Overview of the Fusarium mycotoxins and modified mycotoxins detected in Finnish cereal grains in 2013 (n = 95)
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4446524&req=5

Fig4: Overview of the Fusarium mycotoxins and modified mycotoxins detected in Finnish cereal grains in 2013 (n = 95)
Mentions: The developed and validated LC-MS/MS method was applied for the analysis of 95 cereal grain samples from Finland harvested during 2013, and the results are summarised in Table 4. Figure 4 presents an overview of the detected mycotoxins and modified mycotoxins in barley, oats and wheat. The results of our survey revealed considerable variation between different commodities. The highest contamination of the studied mycotoxins was observed in oats, followed by wheat and barley. The most frequently detected native mycotoxin was DON (incidence 93 % of the samples analysed), followed by NIV (63 %) and HT2 (57 %). DON was also found at the highest concentrations, and particularly in wheat and oats, with 32 % of the analysed oats exceeding the legislative ML of 1750 μg/kg set for DON regarding unprocessed oats placed on the market for first-stage processing [27]. For wheat, the percentage of samples exceeding the ML (1250 μg/kg) was 23 %, whereas no barley sample exceeded the same level. 3Ac-DON (55 %) was only found at increased levels in oats, in samples also showing high concentrations of DON. One wheat and one oat sample also exceeded the ML set for ZEN (100 μg/kg), and both were also highly contaminated with DON (1660 and 23,800 μg/kg, respectively). Such DON levels are unusually high compared to those of previous years based on quantitative results from the Finnish grain quality monitoring programme (1999–2009) [9]. Only minor amounts of HT2 and T2 were detected in barley and wheat. In contrast, the prevalence of these toxins in oats was significantly more pronounced. Nonetheless, only one sample exceeded the indicative value for the sum of these toxins (1000 μg/kg) in Recommendation 2013/165/EU for unprocessed oats [28]. NIV contamination was relatively low in barley and wheat samples in comparison to the levels found in oats, with a mean concentration of 635 μg/kg that can be attributed to four very highly contaminated samples (>1400 μg/kg).Table 4

Bottom Line: Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively.Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing.All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time.

View Article: PubMed Central - PubMed

Affiliation: Chemistry and Toxicology Unit, Research and Laboratory Department, Finnish Food Safety Authority (Evira), Mustialankatu 3, 00790, Helsinki, Finland, alexis.nathanail@helsinki.fi.

ABSTRACT
A reliable and sensitive liquid chromatography-tandem mass spectrometric method was developed for the simultaneous quantitative determination in cereals of the Fusarium mycotoxins HT-2 toxin, T-2 toxin, deoxynivalenol, nivalenol and zearalenone, as well as the modified metabolites 3-acetyl-deoxynivalenol, α-zearalenol, β-zearalenol, deoxynivalenol-3-glucoside, HT-2-3-glucoside, nivalenol-3-glucoside, zearalenone-14-glucoside, zearalenone-14-sulphate, zearalenone-16-glucoside, α-zearalenol-14-glucoside and β-zearalenol-14-glucoside. The 'dilute and shoot' approach was used for sample preparation after extraction with acetonitrile:water:acetic acid (79:20:1, v/v/v). Separation was carried out using reversed-phase liquid chromatography, and detection was performed using tandem mass spectrometry in the selected reaction monitoring mode. The method was in-house validated according to performance characteristics, established in Commission Regulation EC No 401/2006 and Commission Decision EC No 657/2002, prior to its application in a nationwide survey for the analysis of barley, oat and wheat samples (n = 95) harvested in Finland during 2013. Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively. Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing. All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time.

No MeSH data available.


Related in: MedlinePlus