Akihiko Hasegawa

Improved methodology for the simultaneous detection of the trichothecene mycotoxins deoxynivalenol and nivalenol in cereals

A simple and sensitive method has been developed for the analysis of two trichothecene mycotoxins (deoxynivalenol and nivalenol) in cereals. These toxins were extracted with acetonitrile/water (3:1), defatted with n-hexane and purified by a two-step chromatographic procedure using Florisil and Sep-pak columns. The amounts of deoxynivalenol (DON) and nivalenol (NIV) in the column eluates were quantitated by gas chromatography with electron capture detector and gas chromatography-mass spectrometry (selected ion monitoring). The limits of detection of the method were 2.0 micrograms/kg for DON and NIV with recoveries of the toxins spiked into polished rice, wheat and corn at 300 micrograms/kg averaging 87% and 86% respectively.

Rapid and sensitive determination of zearalenone in cereals by high-performance liquid chromatography with fluorescence detection

Zearalenone, an estrogenic mycotoxin of Fusarium species, in cereals can be extracted with acetonitrile-water (3:1), purified on a Florisil column, resolved by high-performance liquid chromatography (HPLC) with a Nucleosil 50-10 column using 90% water-saturated chloroform-cyclohexane-acetonitrile-ethanol (50:15:2:1) and quantitated by fluorescence measurement. This method is rapid, simple and reproducible, and detects zearalenone in wheat, barley, corn and other cereals with picogram sensitivity. A combination of this HPLC method with a gas-liquid chromatographic method for trichothecenes may be applied to the simultaneous detection of Fusarium mycotoxins (zearalenone, nivalenol and deoxynivalenol) in cereals.

A survey of the natural occurrence of Fusarium mycotoxins, deoxynivalenol, nivalenol and zearalenone, in cereals harvested in the Netherlands.

A survey for the natural occurrence of Fusarium mycotoxins, deoxynivalenol (DON), nivalenol (NIV) and zearalenone (ZEN), in Dutch cereals (totaling 29 samples) harvested in 1984/1985, showed that 90%, 79% and 62% of samples were contaminated with DON, NIV and ZEN, respectively. Average contents (ng/g) in the total of positive samples were 221 (DON), 123 (NIV) and 61 (ZEN). Among the cereals examined, the highest concentrations (ng/g) was 3198 (DON), 1875 (NIV) and 677 (ZEN) in a yellow corn sample for animal feed. The results of this survey show that Dutch cereals were relatively significantly contaminated with Fusarium mycotoxins.

The coexistence of the Fusarium mycotoxins nivalenol, deoxynivalenol and zearalenone in Korean cereals harvested in 1983

A survey for the occurrence of nivalenol (NIV), deoxynivalenol (DON) and zearalenone (ZEN) in Korean cereals (totalling 53 samples) harvested in 1983, showed that 96%, 72% and 57% of the samples were contaminated with NIV, DON and ZEN, respectively. Average concentrations (micrograms/kg) in unpolished barley were 546 (NIV), 117 (DON) and 110 (ZEN), and those in polished barley were 130 (NIV) and 21 (DON). The ZEN levels were below the detection limit (1 microgram/kg). Malt, wheat and rye were also heavily contaminated with these Fusarium mycotoxins. The results of this survey show that Korean cereals harvested in 1983 were significantly contaminated with NIV, DON and ZEN, and the incidence and levels, where observed, are similar to those reported in Japan.

A survey of the occurrence of nivalenol, deoxynivalenol and zearalenone in foodstuffs and health foods in Japan

By adopting a rapid and sensitive method for simultaneous detection of nivalenol (NIV), deoxynivalenol (vomitoxin, DON) and zearalenone (ZEN), the natural occurrence of these mycotoxins in Japan in retail marked cereal flours, popcorn and health foods (totalling 76 samples) was surveyed. Significant contamination by NIV and DON was observed in commercial wheat and barley flours, and partially milled grains which are consumed as rice ingredients. Of particular interest was the presence of DON in popcorn imported from the United States, and the high-level contamination of NIV and ZEN in jobs-tears (Hatomugi in Japanese), a widely marketed health food.

A limited survey of Fusarium mycotoxins nivalenol, deoxynivalenol and zearalenone in 1984 UK harvested wheat and barley

A limited survey for the occurrence of nivalenol (NIV), deoxynivalenol (DON) and zearalenone (ZEN) in 1984 UK-grown cereals (31 samples) have been carried out using a new procedure, which is a rapid and sensitive method for Fusarium mycotoxins. NIV, DON and ZEN were detected in 17 (55%), 20 (65%) and 4 (13%) out of 31 samples, and average levels in positive samples were 101 micrograms/kg, 31 micrograms/kg and 1 microgram/kg, respectively. Additional surveys on two wheat and eight barley samples harvested in Scotland have shown that 30%, 60% and 100% of the samples were contaminated with NIV, DON and ZEN, respectively. The contents averaged 391 micrograms/kg of NIV, 39 micrograms/kg of DON and 9 micrograms/kg of ZEN. The results of this survey show that UK-grown cereals were significantly contaminated with NIV, DON and ZEN in a similar way to that observed in Japan, Korea and China. This is the first evidence of the natural occurrence of NIV in UK cereals.

Further survey on the Fusarium mycotoxins in Korean cereals

Fifty-one samples of cereals from the 1984 harvest from Korea were analyzed for nivalenol (NIV), fusarenon-X (FX), deoxynivalenol (DON) and 3-acetyl-DON by gas chromatography (GC) utilizing a 63Ni electron capture detector (ECD), and were quantitated for zearalenone (ZEN) by high-performance liquid chromatography (HPLC) with a fluorescence detector (FD). Trichothecenes and ZEN in the positive samples were confirmed by GC-mass spectrometry (MS). Out of 51 samples, 51, 46 and 42 were positive for NIV, DON and ZEN, respectively, and one malt sample was heavily contaminated with NIV (2675 ng/g) and DON (246 ng/g), and one wheat sample was heavily contaminated with NIV (3169 ng/g). Neither FX nor 3-acetyl-DON was detected in any of the samples. The data reported here indicates that Korean cereals harvested in 1984 are simultaneously contaminated with NIV, DON and ZEN, and the incidences and levels are similar to those observed in the cereals harvested in 1983.

Examination of Chinese and U.S.S.R. cereals for the fusarium mycotoxins, nivalenol, deoxynivalenol and zearalenone

Cereals, foods and feeds sampled in Taiwan, China and the U.S.S.R. were contaminated with nivalenol, deoxynivalenol and zearalenone. The frequencies and levels of contamination are similar to those observed in the cereals of Japan and Korea. This is the first report on the natural occurrence of nivalenol, deoxynivalenol and zearalenone in Chinese and U.S.S.R. cereals, foods and feeds.

A case report on a minor contamination of nivalenol in cereals harvested in Canada

An investigation for the occurrence of nivalenol (NIV), deoxynivalenol (DON) and zearalenone (ZEN) in cereals (ten wheat, one rye and one corn) harvested in Canada have been carried out using a procedure, which is rapid and sensitive for Fusarium mycotoxins. NIV, DON and ZEN were detected in 4, 9 and 9 out of ten wheat samples, and their average levels in the positives were 23 ng/g, 1257 ng/g and 9 ng/g, respectively. One rye and one corn were also contaminated with a minor amount of NIV. This is the first evidence for the natural occurrence of NIV in cereals grown in Canada, though its level was far less than DON.

Comparative determination of free and combined sulphites in foods by the modified rankine method and flame photometric detection gas chromatography. V.

ZusammenfassungEs wurde eine vergleichende Sulfitbestimmung in verschiedenen Lebensmitteln mit Hilfe der modifizierten Rankinemethode (MR), der Gaschromatographie und der Monier-Williams-Methode durchgeführt. Die Ergebnisse stimmen gut überein, wobei die Monier-Williams-Methode geringfügig höhere Werte erbrachte. Diese Methode wird durch schwefelhaltige Lebensmittelinhaltsstoffe empfindlich gestört.Des weiteren wurde in verschiedenen Lebensmitteln die Relation von freiem zu gebundenem Sulfit ermittelt. Dabei stellte sich heraus, daß in den meisten Lebensmitteln 65% des Sulfits in gebundener Form vorliegen. Sowohl MR-Methode als auch Gaschromatographie erlauben eine getrennte Bestimmung von freiem und gebundenem Sulfit. Da beide Methoden einfach und schnell durchzuführen sind, eignen sie sich für die Routinebestimmung.SummaryApplication of the modified Rankine (MR), GLC and present official Monier-Williams methods to the determination of sulphites in a variety of foods was attempted. Generally, sulphite contents determined by these three methods were in good agreement although the values obtained by the modified Monier-Wiliams method were slightly higher than by the other two. A marked interfering effect of other sulphur compounds was observed in the case of determinations by the Monier-Williams method. On the other hand, the determined sulphite values by the MR and GLC methods were independent of the coexisting sulphur compounds. The ratios of free or combined sulphites to total sulphites were compared among the two methods, and in most foods tested the rations of combined to total sulphites were not less than 65%. We conclude that both the MR and GLC methods are valid for the separate determination of free and combined sulphites in most foods, and these two methods will be preferred for routine analysis because of their simplicity and speed.